# 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_DMACuF_c1_s
_database_code_depnum_ccdc_archive 'CCDC 1837735'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c1_s         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.644 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c1_s         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        286 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMACuF_c1_s         
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6

_chemical_name_systematic        'dimethylammonium copper formate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.4292(9)
_cell_length_b                   8.7331(16)
_cell_length_c                   8.8760(14)
_cell_angle_alpha                90
_cell_angle_beta                 96.180(10)
_cell_angle_gamma                90
_cell_volume                     880.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    238
_cell_measurement_theta_min      2.6990
_cell_measurement_theta_max      17.3840

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.558
_shelx_estimated_absorpt_T_min   0.946
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41096
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1405
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.897
_diffrn_reflns_theta_max         20.686
_diffrn_reflns_theta_full        14.275
_diffrn_measured_fraction_theta_max 0.364
_diffrn_measured_fraction_theta_full 0.644
_diffrn_reflns_Laue_measured_fraction_max 0.364
_diffrn_reflns_Laue_measured_fraction_full 0.644
_diffrn_reflns_point_group_measured_fraction_max 0.364
_diffrn_reflns_point_group_measured_fraction_full 0.644
_reflns_number_total             851
_reflns_number_gt                556
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0417P)²+1.1276P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         851
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1340
_refine_ls_wR_factor_gt          0.1030
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0277(3) Uani 1 2 d S . P . .
O2 O 0.3469(2) 0.6033(4) 0.5059(4) 0.0318(7) Uani 1 1 d . . . . .
O1 O 0.4275(3) 0.2329(4) 0.1246(4) 0.0387(8) Uani 1 1 d . . . . .
O3 O 0.4393(3) 0.4114(4) 0.3023(4) 0.0379(8) Uani 1 1 d . . . . .
N1 N 0.250000 0.4361(8) 0.000000 0.0393(14) Uani 1 2 d DS T P . .
H3 H 0.192(4) 0.372(7) -0.056(7) 0.047 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5353(8) 0.500000 0.0277(12) Uani 1 2 d S T P . .
H2 H 0.250000 0.428798 0.499998 0.033 Uiso 1 2 calc R U P . .
C1 C 0.4711(4) 0.2884(6) 0.2473(6) 0.0343(10) Uani 1 1 d . . . . .
H1 H 0.531616 0.234381 0.301960 0.041 Uiso 1 1 calc R U . . .
C3 C 0.1919(6) 0.5284(7) 0.1081(8) 0.0502(15) Uani 1 1 d . . . . .
H4 H 0.155530 0.462008 0.175646 0.060 Uiso 1 1 calc R U . . .
H5 H 0.249066 0.591842 0.165420 0.060 Uiso 1 1 calc R U . . .
H6 H 0.132902 0.591840 0.054031 0.060 Uiso 1 1 calc R U . . .

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
Cu1 0.0168(3) 0.0343(7) 0.0317(7) -0.0042(3) 0.0004(3) 0.0022(2)
O2 0.0202(10) 0.034(2) 0.042(3) 0.0001(12) 0.0032(12) 0.0031(11)
O1 0.0377(15) 0.035(3) 0.042(3) -0.0073(14) -0.0042(15) 0.0026(14)
O3 0.0343(14) 0.046(3) 0.032(3) -0.0085(13) -0.0020(14) 0.0094(14)
N1 0.036(3) 0.030(4) 0.051(5) 0.000 -0.005(3) 0.000
C2 0.021(2) 0.029(4) 0.033(4) 0.000 0.003(2) 0.000
C1 0.0293(17) 0.032(3) 0.041(4) 0.0003(17) -0.0008(18) -0.0010(17)
C3 0.046(3) 0.060(5) 0.047(5) 0.004(3) 0.016(3) 0.010(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
Cu1 O2 1.974(3) . ?
Cu1 O2 1.974(3) 5_666 ?
Cu1 O3 1.974(4) 5_666 ?
Cu1 O3 1.974(4) . ?
O2 C2 1.253(4) . ?
O1 C1 1.246(6) . ?
O3 C1 1.249(6) . ?
N1 C3 1.466(7) . ?
N1 C3 1.466(7) 2 ?
N1 H3 0.97(5) . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.00(17) . 5_666 ?
O2 Cu1 O3 91.41(14) . 5_666 ?
O2 Cu1 O3 88.59(14) 5_666 5_666 ?
O2 Cu1 O3 88.59(14) . . ?
O2 Cu1 O3 91.41(14) 5_666 . ?
O3 Cu1 O3 180.0(2) 5_666 . ?
C2 O2 Cu1 124.3(4) . . ?
C1 O3 Cu1 126.5(3) . . ?
C3 N1 C3 113.3(7) . 2 ?
C3 N1 H3 109(3) . . ?
C3 N1 H3 109(4) 2 . ?
O2 C2 O2 123.4(6) . 2_556 ?
O2 C2 H2 118.3 . . ?
O2 C2 H2 118.3 2_556 . ?
O1 C1 O3 124.8(4) . . ?
O1 C1 H1 117.6 . . ?
O3 C1 H1 117.6 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.523
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.100

_shelx_res_file                  
;
TITL DMACuF_c1_s_a.res in I2/a
    DMACuF_c1_s.res
    created by SHELXL-2016/6 at 12:09:31 on 27-Sep-2017
REM I2/a (#15 in standard setting)
CELL 0.41096   11.429248   8.733127   8.876020    90.0000    96.1796    90.0000
ZERR    4.000   0.000897   0.001602   0.001407     0.0000     0.0102     0.0000
LATT  2
SYMM 1/2-X, Y, -Z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00
L.S. 10
SIZE 0.1 0.04 0.03
ACTA
BOND $H
LIST 4
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.041700    1.127600
FVAR       2.71923
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01676    0.03425 =
         0.03166   -0.00424    0.00039    0.00219
O2    4    0.346939    0.603316    0.505945    11.00000    0.02017    0.03359 =
         0.04159    0.00005    0.00317    0.00308

O1    4    0.427523    0.232891    0.124621    11.00000    0.03775    0.03493 =
         0.04166   -0.00726   -0.00419    0.00264
O3    4    0.439312    0.411382    0.302273    11.00000    0.03426    0.04601 =
         0.03218   -0.00847   -0.00195    0.00944
N1    3    0.250000    0.436060    0.000000    10.50000    0.03568    0.02955 =
         0.05057    0.00000   -0.00491    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.191896    0.371518   -0.055684    11.00000   -1.20000
C2    1    0.250000    0.535289    0.500000    10.50000    0.02101    0.02939 =
         0.03276    0.00000    0.00337    0.00000
AFIX  43
H2    2    0.250000    0.428798    0.499998    10.50000   -1.20000
AFIX   0
C1    1    0.471055    0.288412    0.247292    11.00000    0.02926    0.03167 =
         0.04113    0.00030   -0.00076   -0.00103
AFIX  43
H1    2    0.531616    0.234381    0.301960    11.00000   -1.20000
AFIX   0
C3    1    0.191855    0.528410    0.108107    11.00000    0.04639    0.06012 =
         0.04653    0.00412    0.01598    0.01047
AFIX  33
H4    2    0.155530    0.462008    0.175646    11.00000   -1.20000
H5    2    0.249066    0.591842    0.165420    11.00000   -1.20000
H6    2    0.132902    0.591840    0.054031    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_s_a.res in I2/a
REM R1 =  0.0442 for     556 Fo > 4sig(Fo)  and  0.0668 for all     851 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0412      1.1522

REM Highest difference peak  0.523,  deepest hole -0.813,  1-sigma level  0.100
Q1    1   0.5146  0.5793  0.4149  11.00000  0.05    0.52
Q2    1   0.4495  0.6157  0.4978  11.00000  0.05    0.49
Q3    1   0.5468  0.6172  0.4932  11.00000  0.05    0.44
Q4    1   0.1521  0.3953  0.4916  11.00000  0.05    0.42
Q5    1   0.4278  0.5151  0.5826  11.00000  0.05    0.41
Q6    1   0.5061  0.6558  0.5034  11.00000  0.05    0.40
Q7    1   0.4747  0.5815  0.6016  11.00000  0.05    0.39
Q8    1   0.4303  0.5041  0.2386  11.00000  0.05    0.36
Q9    1   0.5132  0.4954  0.3204  11.00000  0.05    0.32
Q10   1   0.0480  0.4626  0.2470  11.00000  0.05    0.32
Q11   1   0.4707  0.1890  0.0921  11.00000  0.05    0.32
Q12   1   0.5736  0.2706  0.3753  11.00000  0.05    0.32
Q13   1   0.5194  0.1909  0.1250  11.00000  0.05    0.31
Q14   1   0.2500  0.5674  0.0000  10.50000  0.05    0.31
Q15   1   0.4012  0.6129  0.4167  11.00000  0.05    0.30
Q16   1   0.5082  0.2315 -0.0164  11.00000  0.05    0.28
Q17   1   0.4659  0.4378  0.3724  11.00000  0.05    0.28
Q18   1   0.4587  0.2262  0.1961  11.00000  0.05    0.28
Q19   1   0.4108  0.6477  0.5781  11.00000  0.05    0.28
Q20   1   0.3660  0.1169  0.1448  11.00000  0.05    0.27
;
_shelx_res_checksum              24890
####################################################################### 
# 
# 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_DMACuF_c2_p09
_database_code_depnum_ccdc_archive 'CCDC 1837744'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c2_p09       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.549 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_SYMMS02_DMACuF_c2_p09       
;
PROBLEM: No unit-cell angle should be equal to 90 for a triclinic
RESPONSE: This structure forms very close to the transition point, giving  an angle close to 90. Upon further increase in pressure, this angle deviates from 90.
;
_vrf_PLAT043_DMACuF_c2_p09       
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      11.08 Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT911_DMACuF_c2_p09       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        305 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_CHEMW03_DMACuF_c2_p09       
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT041_DMACuF_c2_p09       
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT068_DMACuF_c2_p09       
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT155_DMACuF_c2_p09       
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The cell was kept in the given setting so as to be more comparable to the ambient phase unit cell.
;
_vrf_PLAT202_DMACuF_c2_p09       
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check
RESPONSE: Due to the many parameters in the refinement, refinement of isotropic thermal parameters were preffered.
;
_vrf_PLAT906_DMACuF_c2_p09       
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.200 Check
RESPONSE: The large K value is only observed at the highest resolution of 0.62 Angstrom where the weakest reflections are observed.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4687 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.4601(9)
_cell_length_b                   5.9181(12)
_cell_length_c                   5.784(4)
_cell_angle_alpha                94.58(4)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                96.582(15)
_cell_volume                     185.08(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    71
_cell_measurement_theta_min      4.3470
_cell_measurement_theta_max      12.4330

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_F_000             125
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.665
_shelx_estimated_absorpt_T_min   0.955
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_T_max  1.930
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '5.96 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1072
_diffrn_reflns_av_unetI/netI     0.1503
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.172
_diffrn_reflns_theta_max         19.504
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.382
_diffrn_measured_fraction_theta_full 0.549
_diffrn_reflns_Laue_measured_fraction_max 0.382
_diffrn_reflns_Laue_measured_fraction_full 0.549
_diffrn_reflns_point_group_measured_fraction_max 0.382
_diffrn_reflns_point_group_measured_fraction_full 0.549
_reflns_number_total             1072
_reflns_number_gt                554
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1361P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1072
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0823
_refine_ls_wR_factor_ref         0.2183
_refine_ls_wR_factor_gt          0.2031
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_restrained_S_all      0.908
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0366(8) Uani 1 2 d S . P . .
O1 O 0.632(2) 0.636(3) 0.801(2) 0.034(3) Uiso 0.5 1 d . . P . .
O2 O 0.697(2) 0.590(3) 1.165(3) 0.035(3) Uiso 0.5 1 d . . P . .
O3 O -0.1884(19) 0.613(3) 0.361(3) 0.028(3) Uiso 0.5 1 d . . P . .
O4 O 0.214(2) 0.599(3) 0.366(3) 0.036(3) Uiso 0.5 1 d . . P . .
O5 O 0.338(2) -0.181(3) 0.394(3) 0.038(3) Uiso 0.5 1 d . . P . .
O6 O 0.368(2) 0.192(3) 0.389(3) 0.042(4) Uiso 0.5 1 d . . P . .
C1 C 0.581(2) 0.541(3) 0.982(3) 0.019(4) Uiso 0.5 1 d . . P . .
C3 C 0.440(2) 0.010(5) 0.459(3) 0.028(5) Uiso 0.5 1 d . . P . .
C2 C 0.002(3) 0.547(3) 0.445(3) 0.021(4) Uiso 0.5 1 d . . P . .
C4 C 0.159(2) -0.103(4) 0.919(3) 0.073(4) Uiso 1 1 d . . . . .
N1 N -0.001(3) -0.021(5) 1.080(3) 0.041(4) Uiso 0.5 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0327(10) 0.0423(17) 0.0305(11) -0.0090(15) -0.0065(7) -0.0058(9)

_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
Cu1 O4 1.914(13) . ?
Cu1 O4 1.914(13) 2_666 ?
Cu1 O6 1.940(19) 2_666 ?
Cu1 O6 1.940(19) . ?
Cu1 O3 1.954(12) 2_566 ?
Cu1 O3 1.954(12) 1_655 ?
Cu1 O1 1.958(15) 2_666 ?
Cu1 O1 1.958(15) . ?
Cu1 O2 2.284(16) 2_667 ?
Cu1 O2 2.284(16) 1_554 ?
Cu1 O5 2.298(19) 1_565 ?
Cu1 O5 2.298(19) 2_656 ?
O1 C1 1.24(2) . ?
O1 O6 1.56(2) 2_666 ?
O2 C1 1.23(2) . ?
O2 O3 1.28(2) 1_656 ?
O2 C1 1.80(2) 2_667 ?
O3 C2 1.26(2) . ?
O3 C2 1.90(2) 2_566 ?
O4 C2 1.26(2) . ?
O4 O5 1.39(3) 1_565 ?
O4 C2 1.80(2) 2_566 ?
O5 C3 1.24(3) . ?
O5 C3 1.67(2) 2_656 ?
O6 C3 1.28(3) . ?
C1 C1 0.99(3) 2_667 ?
C3 C3 0.84(3) 2_656 ?
C2 C2 0.88(3) 2_566 ?
C4 N1 1.20(3) 2_557 ?
C4 N1 1.37(3) . ?
N1 N1 0.98(4) 2_557 ?

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
O4 Cu1 O4 180.0(10) . 2_666 ?
O4 Cu1 O6 92.9(7) . 2_666 ?
O4 Cu1 O6 87.1(7) 2_666 2_666 ?
O4 Cu1 O6 87.1(7) . . ?
O4 Cu1 O6 92.9(7) 2_666 . ?
O6 Cu1 O6 180.0 2_666 . ?
O4 Cu1 O3 65.4(6) . 2_566 ?
O4 Cu1 O3 114.6(6) 2_666 2_566 ?
O6 Cu1 O3 115.0(7) 2_666 2_566 ?
O6 Cu1 O3 65.0(7) . 2_566 ?
O4 Cu1 O3 114.6(6) . 1_655 ?
O4 Cu1 O3 65.4(6) 2_666 1_655 ?
O6 Cu1 O3 65.0(7) 2_666 1_655 ?
O6 Cu1 O3 115.0(7) . 1_655 ?
O3 Cu1 O3 180.0 2_566 1_655 ?
O4 Cu1 O1 58.9(7) . 2_666 ?
O4 Cu1 O1 121.1(7) 2_666 2_666 ?
O6 Cu1 O1 133.0(7) 2_666 2_666 ?
O6 Cu1 O1 47.0(7) . 2_666 ?
O3 Cu1 O1 88.3(6) 2_566 2_666 ?
O3 Cu1 O1 91.7(6) 1_655 2_666 ?
O4 Cu1 O1 121.1(7) . . ?
O4 Cu1 O1 58.9(7) 2_666 . ?
O6 Cu1 O1 47.0(7) 2_666 . ?
O6 Cu1 O1 133.0(7) . . ?
O3 Cu1 O1 91.7(6) 2_566 . ?
O3 Cu1 O1 88.3(6) 1_655 . ?
O1 Cu1 O1 180.0 2_666 . ?
O4 Cu1 O2 93.7(6) . 2_667 ?
O4 Cu1 O2 86.3(6) 2_666 2_667 ?
O6 Cu1 O2 96.3(7) 2_666 2_667 ?
O6 Cu1 O2 83.7(7) . 2_667 ?
O3 Cu1 O2 34.1(5) 2_566 2_667 ?
O3 Cu1 O2 145.9(5) 1_655 2_667 ?
O1 Cu1 O2 120.3(5) 2_666 2_667 ?
O1 Cu1 O2 59.7(5) . 2_667 ?
O4 Cu1 O2 86.3(6) . 1_554 ?
O4 Cu1 O2 93.7(6) 2_666 1_554 ?
O6 Cu1 O2 83.7(7) 2_666 1_554 ?
O6 Cu1 O2 96.3(7) . 1_554 ?
O3 Cu1 O2 145.9(5) 2_566 1_554 ?
O3 Cu1 O2 34.1(5) 1_655 1_554 ?
O1 Cu1 O2 59.7(5) 2_666 1_554 ?
O1 Cu1 O2 120.3(6) . 1_554 ?
O2 Cu1 O2 180.0 2_667 1_554 ?
O4 Cu1 O5 37.2(6) . 1_565 ?
O4 Cu1 O5 142.8(7) 2_666 1_565 ?
O6 Cu1 O5 57.0(6) 2_666 1_565 ?
O6 Cu1 O5 123.0(6) . 1_565 ?
O3 Cu1 O5 91.4(6) 2_566 1_565 ?
O3 Cu1 O5 88.6(6) 1_655 1_565 ?
O1 Cu1 O5 83.8(7) 2_666 1_565 ?
O1 Cu1 O5 96.2(7) . 1_565 ?
O2 Cu1 O5 105.3(6) 2_667 1_565 ?
O2 Cu1 O5 74.7(6) 1_554 1_565 ?
O4 Cu1 O5 142.8(7) . 2_656 ?
O4 Cu1 O5 37.2(6) 2_666 2_656 ?
O6 Cu1 O5 123.0(6) 2_666 2_656 ?
O6 Cu1 O5 57.0(6) . 2_656 ?
O3 Cu1 O5 88.6(6) 2_566 2_656 ?
O3 Cu1 O5 91.4(6) 1_655 2_656 ?
O1 Cu1 O5 96.2(7) 2_666 2_656 ?
O1 Cu1 O5 83.8(7) . 2_656 ?
O2 Cu1 O5 74.7(6) 2_667 2_656 ?
O2 Cu1 O5 105.3(6) 1_554 2_656 ?
O5 Cu1 O5 180.0 1_565 2_656 ?
C1 O1 O6 160.2(16) . 2_666 ?
C1 O1 Cu1 121.0(13) . . ?
O6 O1 Cu1 65.9(8) 2_666 . ?
C1 O2 O3 172(2) . 1_656 ?
C1 O2 C1 31.6(13) . 2_667 ?
O3 O2 C1 143.5(14) 1_656 2_667 ?
C1 O2 Cu1 117.4(11) . 1_556 ?
O3 O2 Cu1 58.7(9) 1_656 1_556 ?
C1 O2 Cu1 85.9(7) 2_667 1_556 ?
C2 O3 O2 137.4(17) . 1_454 ?
C2 O3 C2 22.5(12) . 2_566 ?
O2 O3 C2 141.5(17) 1_454 2_566 ?
C2 O3 Cu1 115.4(12) . 1_455 ?
O2 O3 Cu1 87.2(8) 1_454 1_455 ?
C2 O3 Cu1 92.8(9) 2_566 1_455 ?
C2 O4 O5 123.0(19) . 1_565 ?
C2 O4 C2 26.5(12) . 2_566 ?
O5 O4 C2 129.9(15) 1_565 2_566 ?
C2 O4 Cu1 121.4(13) . . ?
O5 O4 Cu1 86.6(8) 1_565 . ?
C2 O4 Cu1 95.0(9) 2_566 . ?
C3 O5 O4 168.8(19) . 1_545 ?
C3 O5 C3 28.7(17) . 2_656 ?
O4 O5 C3 145.2(15) 1_545 2_656 ?
C3 O5 Cu1 119.8(13) . 1_545 ?
O4 O5 Cu1 56.2(10) 1_545 1_545 ?
C3 O5 Cu1 91.1(9) 2_656 1_545 ?
C3 O6 O1 149.4(17) . 2_666 ?
C3 O6 Cu1 124.7(12) . . ?
O1 O6 Cu1 67.1(9) 2_666 . ?
C1 C1 O2 108(3) 2_667 . ?
C1 C1 O1 126(2) 2_667 . ?
O2 C1 O1 123.5(16) . . ?
C1 C1 O2 40.6(17) 2_667 2_667 ?
O2 C1 O2 148.4(13) . 2_667 ?
O1 C1 O2 86.7(11) . 2_667 ?
C3 C3 O5 106(5) 2_656 . ?
C3 C3 O6 132(4) 2_656 . ?
O5 C3 O6 122.0(15) . . ?
C3 C3 O5 45(3) 2_656 2_656 ?
O5 C3 O5 151.3(17) . 2_656 ?
O6 C3 O5 86.7(16) . 2_656 ?
C2 C2 O3 124(3) 2_566 . ?
C2 C2 O4 114(2) 2_566 . ?
O3 C2 O4 122.3(15) . . ?
C2 C2 O4 40.0(18) 2_566 2_566 ?
O3 C2 O4 84.1(11) . 2_566 ?
O4 C2 O4 153.5(12) . 2_566 ?
C2 C2 O3 33.5(17) 2_566 2_566 ?
O3 C2 O3 157.5(12) . 2_566 ?
O4 C2 O3 80.2(11) . 2_566 ?
O4 C2 O3 73.4(9) 2_566 2_566 ?
N1 C4 N1 44.2(17) 2_557 . ?
N1 N1 C4 78(3) 2_557 2_557 ?
N1 N1 C4 58(2) 2_557 . ?
C4 N1 C4 135.8(17) 2_557 . ?

_refine_diff_density_max         1.318
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.164

_shelx_res_file                  
;
TITL DMACuF_c2_p09_s_twin in P-1
    DMACuF_c2_p09_s_twin1_hklf5.res
    created by SHELXL-2016/6 at 15:56:44 on 21-Mar-2018
REM P-1 (#2 in standard setting)
CELL 0.41108  5.460108  5.918063    5.784474    94.5762  89.9975  96.5821
ZERR    1.00  0.000853   0.001183    0.003712   0.0421    0.0348  0.0146
LATT  1
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.14091!source kissel
DISP $H -0.00003  0.00000  0.64127!source kissel
DISP $N  0.00062  0.00099  7.19030!source kissel
DISP $O  0.00180  0.00183 10.15475!source kissel
DISP $Cu  0.24634  0.46870 1129.00277!source kissel
UNIT 5.00 11.00 1.00 6.00 1.00
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 50
SIZE 0.070 0.045 0.020
ACTA
BOND
FMAP 2
PLAN 20
MERG 0
WGHT    0.136100
BASF   0.56621
FVAR      16.78192
MOLE   1
CU1   5    0.500000    0.500000    0.500000    10.50000    0.03265    0.04235 =
         0.03054   -0.00899   -0.00646   -0.00576
O1    4    0.632109    0.635791    0.800624    10.50000    0.03428
O2    4    0.696708    0.590402    1.165421    10.50000    0.03544
O3    4   -0.188366    0.613397    0.361007    10.50000    0.02812
O4    4    0.214216    0.599186    0.366024    10.50000    0.03616
O5    4    0.338159   -0.181428    0.393830    10.50000    0.03800
O6    4    0.368457    0.192011    0.388944    10.50000    0.04186
C1    1    0.581022    0.541291    0.981685    10.50000    0.01895
C3    1    0.439941    0.010488    0.459047    10.50000    0.02775
C2    1    0.001520    0.547296    0.445318    10.50000    0.02124
C4    1    0.159240   -0.102604    0.918843    11.00000    0.07344
N1    3   -0.000541   -0.021266    1.080196    10.50000    0.04138
MOLE   2
HKLF 5 1 0 1 0 1 0 0 0 0 1 1 0




REM  DMACuF_c2_p09_s_twin in P-1
REM R1 =  0.0823 for     554 Fo > 4sig(Fo)  and  0.1251 for all    1072 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.1361      0.0000

REM Highest difference peak  1.318,  deepest hole -1.210,  1-sigma level  0.164
Q1    1   0.3535  0.5143  0.5183  11.00000  0.05    1.32
Q2    1  -0.2736  0.6389  0.5063  11.00000  0.05    0.84
Q3    1   0.5059  0.6662  0.5137  11.00000  0.05    0.76
Q4    1   0.1455 -0.0280  0.8359  11.00000  0.05    0.72
Q5    1   0.4803  0.3564  0.5977  11.00000  0.05    0.71
Q6    1   0.4477  0.4874  0.3295  11.00000  0.05    0.62
Q7    1   0.1780 -0.1856  0.9821  11.00000  0.05    0.61
Q8    1   0.3412  0.5326  0.3484  11.00000  0.05    0.60
Q9    1   0.3626  0.0007  0.4202  11.00000  0.05    0.52
Q10   1   0.7342  0.5336  1.1867  11.00000  0.05    0.47
Q11   1   0.4772  0.5162  0.8208  11.00000  0.05    0.46
Q12   1   0.2097  0.0944  1.1155  11.00000  0.05    0.42
Q13   1   0.8670  0.4939  1.0829  11.00000  0.05    0.42
Q14   1  -0.0076  0.4348  0.3526  11.00000  0.05    0.41
Q15   1   0.2241 -0.1541  0.4204  11.00000  0.05    0.40
Q16   1   0.6990  0.5631  0.7997  11.00000  0.05    0.38
Q17   1   0.0000  0.0000  0.5000  10.50000  0.05    0.38
Q18   1  -0.3517  0.4865  0.3402  11.00000  0.05    0.36
Q19   1   0.9005  0.7174  1.1787  11.00000  0.05    0.35
Q20   1   0.5688  0.4071  0.8703  11.00000  0.05    0.34
;
_shelx_res_checksum              88043
####################################################################### 
# 
# 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_DMAMnF_c3_p02_s
_database_code_depnum_ccdc_archive 'CCDC 1837766'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1791 0.2616 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.26613(19)
_cell_length_b                   8.26613(19)
_cell_length_c                   22.2627(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1317.38(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    277
_cell_measurement_theta_min      2.6790
_cell_measurement_theta_max      16.8820

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.336
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98713
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '1.32 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            799
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.176
_diffrn_reflns_theta_max         19.643
_diffrn_reflns_theta_full        14.283
_diffrn_measured_fraction_theta_max 0.503
_diffrn_measured_fraction_theta_full 0.832
_diffrn_reflns_Laue_measured_fraction_max 0.503
_diffrn_reflns_Laue_measured_fraction_full 0.832
_diffrn_reflns_point_group_measured_fraction_max 0.503
_diffrn_reflns_point_group_measured_fraction_full 0.832
_reflns_number_total             341
_reflns_number_gt                305
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0197P)²+2.0935P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         341
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_restrained_S_all      1.288
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mn1 Mn 0.666667 0.333333 0.333333 0.0240(2) Uani 1 6 d S T P . .
N1 N 0.7504(10) 0.333333 0.083333 0.0400(17) Uani 0.3333 2 d DS T P . .
H3 H 0.763(8) 0.232(5) 0.079(4) 0.048 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0288(2) 0.0585(13) Uani 1 3 d DS T P . .
H2 H 0.554(4) 0.191(2) 0.0217(12) 0.070 Uiso 1 1 d D U . . .
O1 O 0.8733(2) 0.3149(2) 0.27832(6) 0.0384(4) Uani 1 1 d . . . . .
C1 C 1.000000 0.4468(4) 0.250000 0.0317(6) Uani 1 2 d S T P . .
H1 H 0.999999 0.559318 0.249998 0.038 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0245(3) 0.0245(3) 0.0230(3) 0.000 0.000 0.01223(14)
N1 0.033(3) 0.029(3) 0.056(4) -0.009(4) -0.004(2) 0.0147(17)
C2 0.068(2) 0.068(2) 0.0386(18) 0.000 0.000 0.0342(10)
O1 0.0365(8) 0.0348(8) 0.0435(7) 0.0058(8) 0.0147(8) 0.0175(6)
C1 0.0295(13) 0.0295(9) 0.0360(11) 0.0009(7) 0.0017(13) 0.0147(6)

_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
Mn1 O1 2.1683(14) . ?
Mn1 O1 2.1683(14) 31_655 ?
Mn1 O1 2.1683(15) 33_545 ?
Mn1 O1 2.1683(14) 3_665 ?
Mn1 O1 2.1683(14) 32 ?
Mn1 O1 2.1683(14) 2_655 ?
N1 N1 1.199(14) 3_665 ?
N1 N1 1.199(14) 2_655 ?
N1 C2 1.398(6) 16_544 ?
N1 C2 1.398(6) . ?
O1 C1 1.241(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 Mn1 O1 180.00(9) . 31_655 ?
O1 Mn1 O1 88.77(6) . 33_545 ?
O1 Mn1 O1 91.23(6) 31_655 33_545 ?
O1 Mn1 O1 91.23(6) . 3_665 ?
O1 Mn1 O1 88.77(6) 31_655 3_665 ?
O1 Mn1 O1 180.0 33_545 3_665 ?
O1 Mn1 O1 88.77(6) . 32 ?
O1 Mn1 O1 91.23(6) 31_655 32 ?
O1 Mn1 O1 91.23(6) 33_545 32 ?
O1 Mn1 O1 88.77(6) 3_665 32 ?
O1 Mn1 O1 91.23(6) . 2_655 ?
O1 Mn1 O1 88.77(6) 31_655 2_655 ?
O1 Mn1 O1 88.77(6) 33_545 2_655 ?
O1 Mn1 O1 91.23(6) 3_665 2_655 ?
O1 Mn1 O1 180.0 32 2_655 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 64.6(3) 3_665 16_544 ?
N1 N1 C2 64.6(3) 2_655 16_544 ?
N1 N1 C2 64.6(3) 3_665 . ?
N1 N1 C2 64.6(3) 2_655 . ?
C2 N1 C2 120.7(6) 16_544 . ?
N1 C2 N1 50.8(5) . 3_665 ?
N1 C2 N1 50.8(5) . 2_655 ?
N1 C2 N1 50.8(5) 3_665 2_655 ?
C1 O1 Mn1 124.98(16) . . ?
O1 C1 O1 125.7(3) 6_765 . ?

_refine_diff_density_max         0.221
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.057

_shelx_res_file                  
;
TITL DMAMnF_c3_p02_s in R-3c
    DMAMnF_c3_p02_s.res
    created by SHELXL-2016/6 at 10:20:17 on 23-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41119   8.266126   8.266126  22.262671  90.0000  90.0000 120.0000
ZERR    6.00   0.000188   0.000188   0.000326   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Mn
DISP $C -0.00006  0.00048  5.14212!source kissel
DISP $H -0.00003  0.00000  0.64130!source kissel
DISP $N  0.00062  0.00099  7.19266!source kissel
DISP $O  0.00180  0.00183 10.15895!source kissel
DISP $Mn  0.17908  0.26161 636.31605!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT -1 1 4
OMIT -1 2 0
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.019700    2.093500
FVAR       3.35846
MOLE   1
MN1   5    0.666667    0.333333    0.333333    10.16667    0.02445    0.02445 =
         0.02305    0.00000    0.00000    0.01223
N1    3    0.750378    0.333333    0.083333    10.16667    0.03313    0.02946 =
         0.05622   -0.00870   -0.00435    0.01473
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.762908    0.232466    0.079454    10.33333   -1.20000
C2    1    0.666667    0.333333    0.028764    10.33333    0.06843    0.06843 =
         0.03858    0.00000    0.00000    0.03422
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.553621    0.191134    0.021747    11.00000   -1.20000
O1    4    0.873327    0.314904    0.278323    11.00000    0.03648    0.03476 =
         0.04354    0.00581    0.01468    0.01749
C1    1    1.000000    0.446811    0.250000    10.50000    0.02947    0.02951 =
         0.03596    0.00087    0.00174    0.01474
AFIX  43
H1    2    0.999999    0.559318    0.249998    10.50000   -1.20000
AFIX   0
HKLF 4




REM  DMAMnF_c3_p02_s in R-3c
REM R1 =  0.0285 for     305 Fo > 4sig(Fo)  and  0.0327 for all     341 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0200      2.0884

REM Highest difference peak  0.221,  deepest hole -0.320,  1-sigma level  0.057
Q1    1   0.7128  0.3222 -0.0069  11.00000  0.05    0.22
Q2    1   1.0009  0.3003  0.2630  11.00000  0.05    0.20
Q3    1   1.0226  0.5861  0.2822  11.00000  0.05    0.18
Q4    1   0.9656  0.6539  0.2823  11.00000  0.05    0.18
Q5    1   0.8239  0.3566  0.2690  11.00000  0.05    0.17
Q6    1   1.0000  0.6555  0.2500  10.50000  0.05    0.17
Q7    1   1.1071  0.5798  0.2637  11.00000  0.05    0.17
Q8    1   0.6705  0.2100  0.3463  11.00000  0.05    0.17
Q9    1   0.7974  0.3406  0.2928  11.00000  0.05    0.16
Q10   1   0.7390  0.2569  0.0427  11.00000  0.05    0.16
Q11   1   1.0433  0.6557  0.2804  11.00000  0.05    0.16
Q12   1   0.9751  0.3775  0.2973  11.00000  0.05    0.16
Q13   1   0.9143  0.3998  0.3138  11.00000  0.05    0.14
Q14   1   0.7132  0.3779  0.0640  11.00000  0.05    0.14
Q15   1   0.6899  0.1383  0.3068  11.00000  0.05    0.13
Q16   1   0.5264  0.1237 -0.0171  11.00000  0.05    0.12
Q17   1   0.8957  0.2641  0.2891  11.00000  0.05    0.12
Q18   1   0.8567  0.5493  0.2760  11.00000  0.05    0.12
Q19   1   0.6643  0.4604  0.3547  11.00000  0.05    0.12
Q20   1   0.8539  0.2920  0.0476  11.00000  0.05    0.12
;
_shelx_res_checksum              5259


# start Validation Reply Form
_vrf_PLAT029_DMAMnF_c3_p02_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.832 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAMnF_c3_p02_s     
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.86 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAMnF_c3_p02_s     
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.59 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances.  In addition, as the (CH3)2NH2 unit
is dynamically disordered, accurate positioning of the H atoms may not
always be possible.
;
_vrf_PLAT911_DMAMnF_c3_p02_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 43 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMAMnF_c3_p02_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAMnF_c3_p03_s
_database_code_depnum_ccdc_archive 'CCDC 1837767'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1791 0.2616 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.2046(2)
_cell_length_b                   8.2046(2)
_cell_length_c                   21.6892(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1264.41(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    263
_cell_measurement_theta_min      3.3030
_cell_measurement_theta_max      15.7690

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.350
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97391
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '2.56 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            752
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.734
_diffrn_reflns_theta_max         19.501
_diffrn_reflns_theta_full        14.283
_diffrn_measured_fraction_theta_max 0.512
_diffrn_measured_fraction_theta_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.512
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.512
_diffrn_reflns_point_group_measured_fraction_full 0.849
_reflns_number_total             325
_reflns_number_gt                286
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+3.0172P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         325
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0973
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_restrained_S_all      1.228
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mn1 Mn 0.666667 0.333333 0.333333 0.0275(3) Uani 1 6 d S T P . .
N1 N 0.7462(12) 0.333333 0.083333 0.042(2) Uani 0.3333 2 d DS T P . .
H3 H 0.772(8) 0.239(6) 0.082(6) 0.050 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0275(2) 0.0641(19) Uani 1 3 d DS T P . .
H2 H 0.564(5) 0.187(2) 0.0176(17) 0.077 Uiso 1 1 d D U . . .
O1 O 0.8696(3) 0.3076(3) 0.27760(8) 0.0416(5) Uani 1 1 d . . . . .
C1 C 1.000000 0.4429(4) 0.250000 0.0330(7) Uani 1 2 d S T P . .
H1 H 1.000001 0.556222 0.250000 0.040 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0290(4) 0.0290(4) 0.0246(4) 0.000 0.000 0.01449(18)
N1 0.036(3) 0.036(4) 0.053(5) -0.011(5) -0.005(3) 0.018(2)
C2 0.080(3) 0.080(3) 0.032(2) 0.000 0.000 0.0402(15)
O1 0.0393(10) 0.0399(10) 0.0444(9) 0.0054(9) 0.0151(9) 0.0188(8)
C1 0.0326(16) 0.0324(11) 0.0340(13) 0.0002(8) 0.0003(15) 0.0163(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
Mn1 O1 2.1518(18) 31_655 ?
Mn1 O1 2.1518(18) 33_545 ?
Mn1 O1 2.1518(18) . ?
Mn1 O1 2.1519(18) 3_665 ?
Mn1 O1 2.1519(18) 32 ?
Mn1 O1 2.1519(18) 2_655 ?
N1 N1 1.130(17) 3_665 ?
N1 N1 1.130(17) 2_655 ?
N1 C2 1.376(6) 16_544 ?
N1 C2 1.376(6) . ?
O1 C1 1.244(3) . ?

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 Mn1 O1 91.53(7) 31_655 33_545 ?
O1 Mn1 O1 180.0 31_655 . ?
O1 Mn1 O1 88.47(7) 33_545 . ?
O1 Mn1 O1 88.48(7) 31_655 3_665 ?
O1 Mn1 O1 180.0 33_545 3_665 ?
O1 Mn1 O1 91.52(7) . 3_665 ?
O1 Mn1 O1 91.52(7) 31_655 32 ?
O1 Mn1 O1 91.52(7) 33_545 32 ?
O1 Mn1 O1 88.47(7) . 32 ?
O1 Mn1 O1 88.48(7) 3_665 32 ?
O1 Mn1 O1 88.48(7) 31_655 2_655 ?
O1 Mn1 O1 88.48(7) 33_545 2_655 ?
O1 Mn1 O1 91.52(7) . 2_655 ?
O1 Mn1 O1 91.52(7) 3_665 2_655 ?
O1 Mn1 O1 180.0 32 2_655 ?
N1 N1 N1 59.998(1) 3_665 2_655 ?
N1 N1 C2 65.8(3) 3_665 16_544 ?
N1 N1 C2 65.8(3) 2_655 16_544 ?
N1 N1 C2 65.8(3) 3_665 . ?
N1 N1 C2 65.8(3) 2_655 . ?
C2 N1 C2 123.4(8) 16_544 . ?
N1 C2 N1 48.5(7) . 3_665 ?
N1 C2 N1 48.5(7) . 2_655 ?
N1 C2 N1 48.5(7) 3_665 2_655 ?
C1 O1 Mn1 123.0(2) . . ?
O1 C1 O1 124.9(4) 6_765 . ?

_refine_diff_density_max         0.306
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.071

_shelx_res_file                  
;
TITL DMAMnF_c3_p03_s in R-3c
    DMAMnF_c3_p03_s.res
    created by SHELXL-2016/6 at 10:25:20 on 23-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41119   8.204586   8.204586  21.689181  90.0000  90.0000 120.0000
ZERR    6.00   0.000217   0.000217   0.000334   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Mn
DISP $C -0.00006  0.00048  5.14212!source kissel
DISP $H -0.00003  0.00000  0.64130!source kissel
DISP $N  0.00062  0.00099  7.19266!source kissel
DISP $O  0.00180  0.00183 10.15895!source kissel
DISP $Mn  0.17908  0.26161 636.31605!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
TEMP 20
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.035200    3.017200
FVAR       3.49360
MOLE   1
MN1   5    0.666667    0.333333    0.333333    10.16667    0.02899    0.02899 =
         0.02463    0.00000    0.00000    0.01449
N1    3    0.746164    0.333333    0.083333    10.16667    0.03589    0.03611 =
         0.05296   -0.01091   -0.00546    0.01806
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.772216    0.239453    0.081770    10.33333   -1.20000
C2    1    0.666667    0.333333    0.027463    10.33333    0.08040    0.08040 =
         0.03154    0.00000    0.00000    0.04020
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.564032    0.187269    0.017617    11.00000   -1.20000
O1    4    0.869625    0.307599    0.277596    11.00000    0.03927    0.03991 =
         0.04437    0.00539    0.01507    0.01883
C1    1    1.000000    0.442871    0.250000    10.50000    0.03261    0.03242 =
         0.03400    0.00017    0.00034    0.01630
AFIX  43
H1    2    1.000001    0.556222    0.250000    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAMnF_c3_p03_s in R-3c
REM R1 =  0.0369 for     286 Fo > 4sig(Fo)  and  0.0426 for all     325 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0351      3.0180

REM Highest difference peak  0.306,  deepest hole -0.501,  1-sigma level  0.071
Q1    1   0.7902  0.3180  0.3084  11.00000  0.05    0.31
Q2    1   0.6795  0.4769  0.3655  11.00000  0.05    0.26
Q3    1   0.9611  0.3851  0.2969  11.00000  0.05    0.26
Q4    1   0.8620  0.5594  0.2772  11.00000  0.05    0.25
Q5    1   0.9970  0.5827  0.2821  11.00000  0.05    0.23
Q6    1   1.1000  0.5815  0.2633  11.00000  0.05    0.21
Q7    1   0.5720  0.0195  0.0320  11.00000  0.05    0.19
Q8    1   0.6367  0.2614 -0.0126  11.00000  0.05    0.19
Q9    1   0.7059  0.3932  0.3739  11.00000  0.05    0.18
Q10   1   1.1379  0.7049  0.2478  11.00000  0.05    0.16
Q11   1   0.9054  0.4626  0.3087  11.00000  0.05    0.15
Q12   1   0.4010  0.0189  0.0152  11.00000  0.05    0.15
Q13   1   1.0035  0.3283  0.3010  11.00000  0.05    0.15
Q14   1   0.5416  0.2612  0.0170  11.00000  0.05    0.15
Q15   1   1.0290  0.5106  0.2885  11.00000  0.05    0.14
Q16   1   1.0081  0.3002  0.2629  11.00000  0.05    0.14
Q17   1   0.9594  0.6344  0.3134  11.00000  0.05    0.14
Q18   1   0.5173  0.0952 -0.0246  11.00000  0.05    0.14
Q19   1   0.5185  0.2399 -0.0293  11.00000  0.05    0.14
Q20   1   0.7099  0.2391  0.2513  11.00000  0.05    0.14
;
_shelx_res_checksum              97285


# start Validation Reply Form
_vrf_PLAT029_DMAMnF_c3_p03_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.849 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAMnF_c3_p03_s     
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.85 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAMnF_c3_p03_s     
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.72 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances.  In addition, as the (CH3)2NH2 unit
is dynamically disordered, accurate positioning of the H atoms may not
always be possible.
;
_vrf_PLAT911_DMAMnF_c3_p03_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 38 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMAMnF_c3_p03_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMACuF_c1_p02_s
_database_code_depnum_ccdc_archive 'CCDC 1837737'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c1_p02_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.604 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c1_p02_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        307 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT905_DMACuF_c1_p02_s     
;
PROBLEM: Negative K value in the Analysis of Variance ...     -0.077 Report
RESPONSE: The negative K value is only observed at the highest resolution of 0.59 Angstrom where the weakest reflections are observed.
;
_vrf_PLAT978_DMACuF_c1_p02_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.3613(3)
_cell_length_b                   8.6208(5)
_cell_length_c                   8.7180(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.658(3)
_cell_angle_gamma                90
_cell_volume                     849.71(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    269
_cell_measurement_theta_min      1.7150
_cell_measurement_theta_max      17.8330

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.579
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         '0.70 GPa'
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1257
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.718
_diffrn_reflns_theta_max         20.459
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.347
_diffrn_measured_fraction_theta_full 0.604
_diffrn_reflns_Laue_measured_fraction_max 0.347
_diffrn_reflns_Laue_measured_fraction_full 0.604
_diffrn_reflns_point_group_measured_fraction_max 0.347
_diffrn_reflns_point_group_measured_fraction_full 0.604
_reflns_number_total             763
_reflns_number_gt                573
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0251P)²+1.1738P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         763
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0914
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0227(2) Uani 1 2 d S . P . .
O2 O 0.34761(17) 0.6072(3) 0.5062(3) 0.0289(6) Uani 1 1 d . . . . .
O1 O 0.4262(2) 0.2293(4) 0.1212(4) 0.0355(7) Uani 1 1 d . . . . .
O3 O 0.4385(2) 0.4116(3) 0.2990(3) 0.0326(6) Uani 1 1 d . . . . .
N1 N 0.250000 0.4382(6) 0.000000 0.0331(10) Uani 1 2 d DS T P . .
H3 H 0.190(4) 0.373(5) -0.043(6) 0.040 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5385(6) 0.500000 0.0255(9) Uani 1 2 d S T P . .
H2 H 0.250000 0.430658 0.499999 0.031 Uiso 1 2 calc R U P . .
C1 C 0.4699(3) 0.2867(5) 0.2433(5) 0.0309(8) Uani 1 1 d . . . . .
H1 H 0.531028 0.232507 0.298262 0.037 Uiso 1 1 calc R U . . .
C3 C 0.1913(4) 0.5311(6) 0.1087(6) 0.0469(11) Uani 1 1 d . . . . .
H4 H 0.154117 0.463949 0.177395 0.056 Uiso 1 1 calc R U . . .
H5 H 0.248399 0.595329 0.166977 0.056 Uiso 1 1 calc R U . . .
H6 H 0.132430 0.595328 0.053503 0.056 Uiso 1 1 calc R U . . .

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
Cu1 0.0148(2) 0.0297(5) 0.0229(5) -0.00315(17) -0.0016(2) 0.00161(18)
O2 0.0175(7) 0.0304(19) 0.038(2) -0.0022(9) -0.0020(10) -0.0013(9)
O1 0.0335(10) 0.037(2) 0.034(2) -0.0097(10) -0.0049(12) 0.0016(11)
O3 0.0296(9) 0.039(2) 0.028(2) -0.0060(9) -0.0047(11) 0.0063(10)
N1 0.0268(15) 0.031(3) 0.040(3) 0.000 -0.0050(19) 0.000
C2 0.0165(13) 0.030(3) 0.030(3) 0.000 0.0000(17) 0.000
C1 0.0234(11) 0.031(3) 0.037(3) -0.0033(13) 0.0000(14) -0.0001(14)
C3 0.046(2) 0.052(4) 0.044(4) 0.0042(18) 0.013(2) 0.006(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
Cu1 O2 1.968(2) 5_666 ?
Cu1 O2 1.968(2) . ?
Cu1 O3 1.974(3) . ?
Cu1 O3 1.974(3) 5_666 ?
Cu1 O1 2.429(3) 4 ?
Cu1 O1 2.429(3) 8 ?
O2 C2 1.254(3) . ?
O1 C1 1.233(5) . ?
O3 C1 1.248(5) . ?
N1 C3 1.452(5) 2 ?
N1 C3 1.452(5) . ?
N1 H3 0.94(4) . ?
N1 H3 0.94(4) 2 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 5_666 . ?
O2 Cu1 O3 91.70(10) 5_666 . ?
O2 Cu1 O3 88.30(10) . . ?
O2 Cu1 O3 88.30(10) 5_666 5_666 ?
O2 Cu1 O3 91.70(10) . 5_666 ?
O3 Cu1 O3 180.0 . 5_666 ?
O2 Cu1 O1 91.61(10) 5_666 4 ?
O2 Cu1 O1 88.40(10) . 4 ?
O3 Cu1 O1 92.01(11) . 4 ?
O3 Cu1 O1 87.99(11) 5_666 4 ?
O2 Cu1 O1 88.39(10) 5_666 8 ?
O2 Cu1 O1 91.60(10) . 8 ?
O3 Cu1 O1 87.99(11) . 8 ?
O3 Cu1 O1 92.01(11) 5_666 8 ?
O1 Cu1 O1 180.0 4 8 ?
C2 O2 Cu1 123.6(3) . . ?
C1 O1 Cu1 125.1(2) . 4_545 ?
C1 O3 Cu1 126.1(2) . . ?
C3 N1 C3 113.1(5) 2 . ?
C3 N1 H3 116(3) 2 . ?
C3 N1 H3 103(3) . . ?
C3 N1 H3 103(3) 2 2 ?
C3 N1 H3 116(3) . 2 ?
H3 N1 H3 106(6) . 2 ?
O2 C2 O2 123.6(5) . 2_556 ?
O2 C2 H2 118.2 . . ?
O2 C2 H2 118.2 2_556 . ?
O1 C1 O3 125.2(3) . . ?
O1 C1 H1 117.4 . . ?
O3 C1 H1 117.4 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.318
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.093

_shelx_res_file                  
;
TITL DMACuF_c1_p02_s in I2/a
    DMACuF_c1_p02_s.res
    created by SHELXL-2016/6 at 18:20:28 on 16-Apr-2018
REM I2/a (#15 in standard setting)
CELL 0.41108  11.361275   8.620783   8.718014  90.0000  95.6580  90.0000
ZERR    4.00   0.000261   0.000511   0.000490   0.0000   0.0032   0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00

OMIT -9 4 1

L.S. 50
SIZE 0.06 0.04 0.03
ACTA
BOND $H
LIST 4
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.025100    1.173800
FVAR       2.87698
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01481    0.02967 =
         0.02287   -0.00315   -0.00163    0.00161
O2    4    0.347615    0.607213    0.506196    11.00000    0.01749    0.03039 =
         0.03776   -0.00217   -0.00196   -0.00132

O1    4    0.426234    0.229253    0.121170    11.00000    0.03350    0.03722 =
         0.03406   -0.00973   -0.00485    0.00159
O3    4    0.438513    0.411631    0.299022    11.00000    0.02961    0.03876 =
         0.02796   -0.00604   -0.00472    0.00628
N1    3    0.250000    0.438179    0.000000    10.50000    0.02676    0.03111 =
         0.03967    0.00000   -0.00495    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.190010    0.372643   -0.043078    11.00000   -1.20000
C2    1    0.250000    0.538537    0.500000    10.50000    0.01651    0.02994 =
         0.02956    0.00000    0.00000    0.00000
AFIX  43
H2    2    0.250000    0.430658    0.499999    10.50000   -1.20000
AFIX   0
C1    1    0.469862    0.286655    0.243279    11.00000    0.02343    0.03144 =
         0.03732   -0.00335    0.00002   -0.00006
AFIX  43
H1    2    0.531028    0.232507    0.298262    11.00000   -1.20000
AFIX   0
C3    1    0.191259    0.531067    0.108677    11.00000    0.04621    0.05179 =
         0.04441    0.00417    0.01308    0.00551
AFIX  33
H4    2    0.154117    0.463949    0.177395    11.00000   -1.20000
H5    2    0.248399    0.595329    0.166977    11.00000   -1.20000
H6    2    0.132430    0.595328    0.053503    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_p02_s in I2/a
REM R1 =  0.0330 for     573 Fo > 4sig(Fo)  and  0.0470 for all     763 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0251      1.1738

REM Highest difference peak  0.318,  deepest hole -0.395,  1-sigma level  0.093
Q1    1   0.1284  0.5073  0.0107  11.00000  0.05    0.32
Q2    1   0.2500  0.5682  0.0000  10.50000  0.05    0.30
Q3    1   0.1123  0.4780  0.1044  11.00000  0.05    0.30
Q4    1   0.1380  0.5332  0.0914  11.00000  0.05    0.30
Q5    1   0.0848  0.4776  0.0766  11.00000  0.05    0.29
Q6    1   0.0818  0.5210  0.0248  11.00000  0.05    0.27
Q7    1   0.1821  0.6141  0.1964  11.00000  0.05    0.27
Q8    1   0.2105  0.5038 -0.1006  11.00000  0.05    0.27
Q9    1   0.0971  0.3845 -0.0560  11.00000  0.05    0.25
Q10   1   0.5030  0.0960  0.4176  11.00000  0.05    0.25
Q11   1   0.4941  0.3235  0.2000  11.00000  0.05    0.24
Q12   1   0.0227  0.5320  0.1081  11.00000  0.05    0.24
Q13   1   0.1817  0.4371  0.2185  11.00000  0.05    0.24
Q14   1   0.1971  0.6445  0.1253  11.00000  0.05    0.23
Q15   1   0.0234  0.5424 -0.0084  11.00000  0.05    0.23
Q16   1   0.1960  0.5561 -0.0392  11.00000  0.05    0.23
Q17   1   0.4508  0.3586  0.3333  11.00000  0.05    0.22
Q18   1   0.2239  0.3706  0.1737  11.00000  0.05    0.22
Q19   1   0.5673  0.2675  0.3850  11.00000  0.05    0.21
Q20   1   0.4277  0.6783  0.5583  11.00000  0.05    0.21
;
_shelx_res_checksum              12425
####################################################################### 
# 
# 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_DMACuF_c2_p08
_database_code_depnum_ccdc_archive 'CCDC 1837743'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c2_p08       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.562 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c2_p08       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        298 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT353_DMACuF_c2_p08       
;
PROBLEM: Long   N-H (N0.87,N1.01A)  N1       - H3       .       1.03 Ang.
RESPONSE: Only restraints are applied on the N-H bonding length, so the H position may vary depending on the data quality.
;
_vrf_PLAT353_DMACuF_c2_p08_2     
;
PROBLEM: Long   N-H (N0.87,N1.01A)  N1       - H3_j     .       1.03 Ang.
RESPONSE: Only restraints are applied on the N-H bonding length, so the H position may vary depending on the data quality.
;
_vrf_PLAT978_DMACuF_c2_p08       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   10.9738(6)
_cell_length_b                   8.4692(11)
_cell_length_c                   8.1090(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.187(7)
_cell_angle_gamma                90
_cell_volume                     751.64(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    204
_cell_measurement_theta_min      3.0250
_cell_measurement_theta_max      15.3630

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.654
_shelx_estimated_absorpt_T_min   0.932
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_pressure         '5.32 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1121
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.759
_diffrn_reflns_theta_max         20.682
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.327
_diffrn_measured_fraction_theta_full 0.562
_diffrn_reflns_Laue_measured_fraction_max 0.327
_diffrn_reflns_Laue_measured_fraction_full 0.562
_diffrn_reflns_point_group_measured_fraction_max 0.327
_diffrn_reflns_point_group_measured_fraction_full 0.562
_reflns_number_total             656
_reflns_number_gt                469
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²+3.8960P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         656
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1076
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0241(3) Uani 1 2 d S . P . .
O2 O 0.3501(3) 0.6218(5) 0.5072(5) 0.0291(8) Uani 1 1 d . . . . .
O1 O 0.4159(3) 0.2171(5) 0.1117(6) 0.0357(9) Uani 1 1 d . . . . .
O3 O 0.4344(3) 0.4152(5) 0.2867(6) 0.0347(9) Uani 1 1 d . . . . .
N1 N 0.250000 0.4456(10) 0.000000 0.0424(18) Uani 1 2 d DS T P . .
H3 H 0.193(5) 0.357(9) -0.045(10) 0.051 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5522(8) 0.500000 0.0239(12) Uani 1 2 d S T P . .
H2 H 0.250001 0.442407 0.500003 0.029 Uiso 1 2 calc R U P . .
C1 C 0.4627(4) 0.2820(6) 0.2383(7) 0.0291(10) Uani 1 1 d . . . . .
H1 H 0.522937 0.227048 0.301158 0.035 Uiso 1 1 calc R U . . .
C3 C 0.1811(6) 0.5377(9) 0.1085(10) 0.0514(17) Uani 1 1 d . . . . .
H4 H 0.137372 0.468698 0.177212 0.062 Uiso 1 1 calc R U . . .
H5 H 0.235549 0.603123 0.176644 0.062 Uiso 1 1 calc R U . . .
H6 H 0.124086 0.603123 0.044211 0.062 Uiso 1 1 calc R U . . .

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
Cu1 0.0196(4) 0.0310(7) 0.0210(6) -0.0022(3) -0.0045(3) 0.0009(3)
O2 0.0219(12) 0.031(2) 0.035(3) -0.0003(12) 0.0005(14) 0.0014(13)
O1 0.0351(15) 0.043(3) 0.028(3) -0.0062(14) -0.0060(16) -0.0007(16)
O3 0.0335(15) 0.038(3) 0.031(3) -0.0049(14) -0.0095(16) 0.0043(16)
N1 0.038(3) 0.036(5) 0.051(6) 0.000 -0.010(3) 0.000
C2 0.023(2) 0.023(4) 0.025(5) 0.000 -0.001(2) 0.000
C1 0.0283(18) 0.030(3) 0.028(3) -0.0018(16) -0.0037(19) 0.0020(19)
C3 0.055(3) 0.068(6) 0.033(5) 0.010(3) 0.017(3) 0.000(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
Cu1 O2 1.946(3) 5_666 ?
Cu1 O2 1.946(3) . ?
Cu1 O3 1.960(4) . ?
Cu1 O3 1.960(4) 5_666 ?
Cu1 O1 2.275(4) 4 ?
Cu1 O1 2.275(4) 8 ?
O2 C2 1.244(5) . ?
O1 C1 1.242(6) . ?
O3 C1 1.241(6) . ?
N1 C3 1.432(9) 2 ?
N1 C3 1.432(9) . ?
N1 H3 1.02(6) . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 5_666 . ?
O2 Cu1 O3 92.05(16) 5_666 . ?
O2 Cu1 O3 87.95(16) . . ?
O2 Cu1 O3 87.95(16) 5_666 5_666 ?
O2 Cu1 O3 92.05(16) . 5_666 ?
O3 Cu1 O3 180.0 . 5_666 ?
O2 Cu1 O1 92.77(15) 5_666 4 ?
O2 Cu1 O1 87.23(15) . 4 ?
O3 Cu1 O1 94.47(18) . 4 ?
O3 Cu1 O1 85.53(18) 5_666 4 ?
O2 Cu1 O1 87.23(15) 5_666 8 ?
O2 Cu1 O1 92.77(15) . 8 ?
O3 Cu1 O1 85.53(18) . 8 ?
O3 Cu1 O1 94.47(18) 5_666 8 ?
O1 Cu1 O1 180.0 4 8 ?
C2 O2 Cu1 119.5(4) . . ?
C1 O1 Cu1 122.1(3) . 4_545 ?
C1 O3 Cu1 121.9(3) . . ?
C3 N1 C3 114.0(9) 2 . ?
C3 N1 H3 121(5) 2 . ?
C3 N1 H3 107(4) . . ?
O2 C2 O2 123.4(7) 2_556 . ?
O2 C2 H2 118.3 2_556 . ?
O2 C2 H2 118.3 . . ?
O3 C1 O1 124.5(5) . . ?
O3 C1 H1 117.7 . . ?
O1 C1 H1 117.7 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.718
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.104

_shelx_res_file                  
;
TITL DMACuF_c2_p08_s in I2/a
    DMACuF_c2_p08_s_nosg.res
    created by SHELXL-2016/6 at 13:50:26 on 27-Sep-2017
REM I2/a (#15 in standard setting)
CELL 0.41108  10.973799   8.469184   8.109043    90.0000    94.1870    90.0000
ZERR    4.00   0.000564   0.001057   0.000939     0.0000     0.0069     0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00

L.S. 10
SIZE 0.11 0.05 0.03
ACTA
BOND $H
LIST 4
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.041500    3.896000
FVAR       2.59923
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01958    0.03101 =
         0.02096   -0.00225   -0.00451    0.00094
O2    4    0.350112    0.621844    0.507244    11.00000    0.02189    0.03061 =
         0.03460   -0.00030    0.00046    0.00141

O1    4    0.415915    0.217113    0.111747    11.00000    0.03506    0.04250 =
         0.02844   -0.00622   -0.00599   -0.00067
O3    4    0.434449    0.415246    0.286736    11.00000    0.03347    0.03817 =
         0.03085   -0.00493   -0.00945    0.00431
N1    3    0.250000    0.445583    0.000000    10.50000    0.03824    0.03576 =
         0.05141    0.00000   -0.00974    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.193373    0.357388   -0.045275    11.00000   -1.20000
C2    1    0.250000    0.552217    0.500000    10.50000    0.02306    0.02317 =
         0.02521    0.00000   -0.00054    0.00000
AFIX  43
H2    2    0.250001    0.442407    0.500003    10.50000   -1.20000
AFIX   0
C1    1    0.462653    0.282027    0.238316    11.00000    0.02832    0.03012 =
         0.02790   -0.00176   -0.00367    0.00196
AFIX  43
H1    2    0.522937    0.227048    0.301158    11.00000   -1.20000
AFIX   0
C3    1    0.181068    0.537730    0.108460    11.00000    0.05526    0.06799 =
         0.03294    0.01003    0.01712    0.00032
AFIX  33
H4    2    0.137372    0.468698    0.177212    11.00000   -1.20000
H5    2    0.235549    0.603123    0.176644    11.00000   -1.20000
H6    2    0.124086    0.603123    0.044211    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c2_p08_s in I2/a
REM R1 =  0.0442 for     469 Fo > 4sig(Fo)  and  0.0623 for all     656 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0414      3.9047

REM Highest difference peak  0.718,  deepest hole -0.602,  1-sigma level  0.104
Q1    1   0.5789  0.5019  0.4940  11.00000  0.05    0.72
Q2    1   0.5718  0.5536  0.4342  11.00000  0.05    0.49
Q3    1   0.2500  0.5835  0.0000  10.50000  0.05    0.46
Q4    1   0.5207  0.5645  0.5905  11.00000  0.05    0.42
Q5    1   0.3528  0.2028  0.1501  11.00000  0.05    0.41
Q6    1   0.4306  0.5819  0.2961  11.00000  0.05    0.38
Q7    1   0.1520  0.3794  0.4809  11.00000  0.05    0.35
Q8    1   0.4908  0.1111  0.3269  11.00000  0.05    0.34
Q9    1   0.5150  0.4317  0.5721  11.00000  0.05    0.32
Q10   1   0.3566  0.5213  0.5046  11.00000  0.05    0.31
Q11   1   0.3386  0.6731  0.4554  11.00000  0.05    0.31
Q12   1   0.3648  0.3942  0.2888  11.00000  0.05    0.31
Q13   1   0.4380  0.5129  0.2115  11.00000  0.05    0.30
Q14   1   0.3869  0.4865  0.6340  11.00000  0.05    0.30
Q15   1   0.5868  0.3011  0.3966  11.00000  0.05    0.29
Q16   1   0.1817  0.3791  0.2688  11.00000  0.05    0.29
Q17   1   0.2520  0.7179  0.6075  11.00000  0.05    0.29
Q18   1   0.4318  0.5682  0.5738  11.00000  0.05    0.28
Q19   1   0.4386  0.3150  0.1397  11.00000  0.05    0.28
Q20   1   0.4551  0.4642  0.2319  11.00000  0.05    0.28
;
_shelx_res_checksum              46857
####################################################################### 
# 
# 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_DMACuF_c1_p01_s
_database_code_depnum_ccdc_archive 'CCDC 1837736'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c1_p01_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.591 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c1_p01_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        323 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMACuF_c1_p01_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.39538(18)
_cell_length_b                   8.6694(4)
_cell_length_c                   8.7825(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.884(2)
_cell_angle_gamma                90
_cell_volume                     863.06(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    258
_cell_measurement_theta_min      1.7120
_cell_measurement_theta_max      18.2700

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.570
_shelx_estimated_absorpt_T_min   0.967
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         '0.33 GPa'
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1235
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.710
_diffrn_reflns_theta_max         20.416
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.344
_diffrn_measured_fraction_theta_full 0.591
_diffrn_reflns_Laue_measured_fraction_max 0.344
_diffrn_reflns_Laue_measured_fraction_full 0.591
_diffrn_reflns_point_group_measured_fraction_max 0.344
_diffrn_reflns_point_group_measured_fraction_full 0.591
_reflns_number_total             761
_reflns_number_gt                570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0296P)²+0.6842P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         761
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.1008
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0222(2) Uani 1 2 d S . P . .
O2 O 0.34732(17) 0.6054(3) 0.5056(3) 0.0289(6) Uani 1 1 d . . . . .
O1 O 0.4273(2) 0.2313(4) 0.1218(4) 0.0348(7) Uani 1 1 d . . . . .
O3 O 0.4388(2) 0.4119(3) 0.3007(3) 0.0325(7) Uani 1 1 d . . . . .
N1 N 0.250000 0.4371(6) 0.000000 0.0333(10) Uani 1 2 d DS T P . .
H3 H 0.202(4) 0.374(6) -0.046(6) 0.040 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5369(6) 0.500000 0.0237(9) Uani 1 2 d S T P . .
H2 H 0.250000 0.429619 0.500000 0.028 Uiso 1 2 calc R U P . .
C1 C 0.4707(3) 0.2879(5) 0.2450(5) 0.0292(8) Uani 1 1 d . . . . .
H1 H 0.531662 0.233912 0.299863 0.035 Uiso 1 1 calc R U . . .
C3 C 0.1914(4) 0.5296(6) 0.1083(6) 0.0469(11) Uani 1 1 d . . . . .
H4 H 0.154487 0.462704 0.176385 0.056 Uiso 1 1 calc R U . . .
H5 H 0.248400 0.593478 0.166383 0.056 Uiso 1 1 calc R U . . .
H6 H 0.132547 0.593482 0.053487 0.056 Uiso 1 1 calc R U . . .

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
Cu1 0.0141(2) 0.0293(5) 0.0224(5) -0.00320(17) -0.0018(2) 0.00167(17)
O2 0.0165(7) 0.0338(19) 0.036(2) -0.0033(9) 0.0000(9) -0.0008(9)
O1 0.0329(10) 0.039(2) 0.031(2) -0.0103(11) -0.0038(12) 0.0036(11)
O3 0.0281(9) 0.042(2) 0.026(2) -0.0055(10) -0.0054(11) 0.0086(10)
N1 0.0290(16) 0.033(3) 0.036(3) 0.000 -0.007(2) 0.000
C2 0.0142(13) 0.032(3) 0.025(3) 0.000 0.0044(16) 0.000
C1 0.0227(11) 0.032(3) 0.032(3) -0.0009(12) -0.0015(14) 0.0001(14)
C3 0.044(2) 0.057(4) 0.042(4) 0.0021(19) 0.017(2) 0.006(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
Cu1 O2 1.970(2) 5_666 ?
Cu1 O2 1.970(2) . ?
Cu1 O3 1.971(3) 5_666 ?
Cu1 O3 1.971(3) . ?
O2 C2 1.254(3) . ?
O1 C1 1.243(5) . ?
O3 C1 1.251(5) . ?
N1 C3 1.458(6) . ?
N1 C3 1.458(6) 2 ?
N1 H3 0.85(4) . ?
N1 H3 0.85(4) 2 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 5_666 . ?
O2 Cu1 O3 88.22(10) 5_666 5_666 ?
O2 Cu1 O3 91.78(10) . 5_666 ?
O2 Cu1 O3 91.78(10) 5_666 . ?
O2 Cu1 O3 88.22(10) . . ?
O3 Cu1 O3 180.0 5_666 . ?
C2 O2 Cu1 124.0(3) . . ?
C1 O3 Cu1 126.1(2) . . ?
C3 N1 C3 113.2(6) . 2 ?
C3 N1 H3 110(4) . . ?
C3 N1 H3 111(4) 2 . ?
C3 N1 H3 111(4) . 2 ?
C3 N1 H3 110(4) 2 2 ?
H3 N1 H3 99(7) . 2 ?
O2 C2 O2 123.5(5) . 2_556 ?
O2 C2 H2 118.2 . . ?
O2 C2 H2 118.2 2_556 . ?
O1 C1 O3 125.0(3) . . ?
O1 C1 H1 117.5 . . ?
O3 C1 H1 117.5 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.306
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.075

_shelx_res_file                  
;
TITL DMACuF_c1_p01_s in I2/a
    DMACuF_c1_p01_s.res
    created by SHELXL-2016/6 at 12:12:39 on 27-Sep-2017
REM I2/a (#15 in standard setting)
CELL 0.41108  11.395378   8.669376   8.782490  90.0000  95.8843  90.0000
ZERR    4.00   0.000180   0.000371   0.000374   0.0000   0.0024   0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00
L.S. 10
SIZE 0.06 0.04 0.03
ACTA
BOND $H
LIST 2
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.029600    0.684200
FVAR       2.91383
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01407    0.02929 =
         0.02237   -0.00320   -0.00180    0.00167
O2    4    0.347324    0.605358    0.505622    11.00000    0.01652    0.03381 =
         0.03574   -0.00333    0.00001   -0.00081

O1    4    0.427326    0.231266    0.121829    11.00000    0.03293    0.03909 =
         0.03103   -0.01031   -0.00375    0.00357
O3    4    0.438780    0.411897    0.300657    11.00000    0.02808    0.04200 =
         0.02579   -0.00547   -0.00541    0.00857
N1    3    0.250000    0.437082    0.000000    10.50000    0.02899    0.03302 =
         0.03575    0.00000   -0.00678    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.202072    0.373833   -0.045828    11.00000   -1.20000
C2    1    0.250000    0.536893    0.500000    10.50000    0.01422    0.03192 =
         0.02544    0.00000    0.00440    0.00000
AFIX  43
H2    2    0.250000    0.429619    0.500000    10.50000   -1.20000
AFIX   0
C1    1    0.470740    0.287899    0.244957    11.00000    0.02272    0.03168 =
         0.03234   -0.00094   -0.00148    0.00012
AFIX  43
H1    2    0.531662    0.233912    0.299863    11.00000   -1.20000
AFIX   0
C3    1    0.191352    0.529582    0.108308    11.00000    0.04440    0.05693 =
         0.04190    0.00211    0.01695    0.00573
AFIX  33
H4    2    0.154487    0.462704    0.176385    11.00000   -1.20000
H5    2    0.248400    0.593478    0.166383    11.00000   -1.20000
H6    2    0.132547    0.593482    0.053487    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_p01_s in I2/a
REM R1 =  0.0335 for     570 Fo > 4sig(Fo)  and  0.0480 for all     761 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0297      0.6854

REM Highest difference peak  0.306,  deepest hole -0.345,  1-sigma level  0.075
Q1    1   0.1919  0.4883  0.6532  11.00000  0.05    0.31
Q2    1   0.4365  0.5822  0.3027  11.00000  0.05    0.30
Q3    1   0.5704  0.2788  0.3882  11.00000  0.05    0.29
Q4    1   0.2422  0.3886 -0.1028  11.00000  0.05    0.27
Q5    1   0.2987  0.6313  0.5749  11.00000  0.05    0.26
Q6    1   0.2500  0.5963  0.0000  10.50000  0.05    0.26
Q7    1   0.5043  0.3709  0.3349  11.00000  0.05    0.25
Q8    1   0.4998  0.5678  0.4350  11.00000  0.05    0.25
Q9    1   0.4526  0.2196 -0.0582  11.00000  0.05    0.25
Q10   1   0.4114  0.6368  0.5416  11.00000  0.05    0.25
Q11   1   0.1510  0.3985  0.4824  11.00000  0.05    0.24
Q12   1   0.4706  0.3772  0.3221  11.00000  0.05    0.24
Q13   1   0.3468  0.5530  0.5938  11.00000  0.05    0.23
Q14   1   0.4102  0.3891  0.3998  11.00000  0.05    0.23
Q15   1   0.5294  0.5007  0.3431  11.00000  0.05    0.22
Q16   1   0.4455  0.0608  0.1979  11.00000  0.05    0.22
Q17   1   0.1385  0.5401  0.0858  11.00000  0.05    0.22
Q18   1   0.4777  0.6518  0.4823  11.00000  0.05    0.21
Q19   1   0.4487  0.2653  0.0163  11.00000  0.05    0.20
Q20   1   0.1776  0.5935  0.1890  11.00000  0.05    0.20
;
_shelx_res_checksum              73502
####################################################################### 
# 
# 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_DMACuF_c1_p04_s
_database_code_depnum_ccdc_archive 'CCDC 1837739'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c1_p04_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.598 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c1_p04_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        299 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMACuF_c1_p04_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.27196(14)
_cell_length_b                   8.5295(3)
_cell_length_c                   8.5611(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.1904(17)
_cell_angle_gamma                90
_cell_volume                     819.72(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    250
_cell_measurement_theta_min      3.2220
_cell_measurement_theta_max      17.2760

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.600
_shelx_estimated_absorpt_T_min   0.965
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         '1.78 GPa'
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1219
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.734
_diffrn_reflns_theta_max         20.671
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.337
_diffrn_measured_fraction_theta_full 0.598
_diffrn_reflns_Laue_measured_fraction_max 0.337
_diffrn_reflns_Laue_measured_fraction_full 0.598
_diffrn_reflns_point_group_measured_fraction_max 0.337
_diffrn_reflns_point_group_measured_fraction_full 0.598
_reflns_number_total             736
_reflns_number_gt                556
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+1.7070P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         736
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0837
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0243(2) Uani 1 2 d S . P . .
O2 O 0.34801(19) 0.6116(3) 0.5076(4) 0.0321(6) Uani 1 1 d . . . . .
O1 O 0.4245(2) 0.2255(4) 0.1178(4) 0.0362(7) Uani 1 1 d . . . . .
O3 O 0.4377(2) 0.4132(4) 0.2952(4) 0.0355(7) Uani 1 1 d . . . . .
N1 N 0.250000 0.4396(7) 0.000000 0.0363(11) Uani 1 2 d DS T P . .
H3 H 0.197(4) 0.381(6) -0.047(6) 0.044 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5428(7) 0.500000 0.0264(10) Uani 1 2 d S T P . .
H2 H 0.249999 0.433743 0.499999 0.032 Uiso 1 2 calc R U P . .
C1 C 0.4688(3) 0.2847(5) 0.2407(5) 0.0315(8) Uani 1 1 d . . . . .
H1 H 0.529724 0.229927 0.297314 0.038 Uiso 1 1 calc R U . . .
C3 C 0.1896(4) 0.5329(6) 0.1099(7) 0.0490(12) Uani 1 1 d . . . . .
H4 H 0.151454 0.464898 0.179398 0.059 Uiso 1 1 calc R U . . .
H5 H 0.246529 0.597872 0.169793 0.059 Uiso 1 1 calc R U . . .
H6 H 0.130837 0.597871 0.053454 0.059 Uiso 1 1 calc R U . . .

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
Cu1 0.0169(2) 0.0332(5) 0.0221(5) -0.00242(19) -0.0022(2) 0.0017(2)
O2 0.0200(9) 0.036(2) 0.039(2) -0.0016(10) -0.0028(11) 0.0001(10)
O1 0.0350(12) 0.039(2) 0.033(2) -0.0090(11) -0.0059(12) 0.0049(12)
O3 0.0314(11) 0.045(2) 0.029(2) -0.0074(11) -0.0065(12) 0.0099(12)
N1 0.0278(17) 0.035(4) 0.044(4) 0.000 -0.009(2) 0.000
C2 0.0181(15) 0.033(3) 0.028(4) 0.000 -0.0004(18) 0.000
C1 0.0236(12) 0.035(3) 0.034(3) -0.0026(13) -0.0044(15) 0.0018(14)
C3 0.046(2) 0.061(4) 0.041(4) 0.005(2) 0.010(2) 0.003(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
Cu1 O2 1.966(2) . ?
Cu1 O2 1.966(2) 5_666 ?
Cu1 O3 1.973(3) . ?
Cu1 O3 1.973(3) 5_666 ?
Cu1 O1 2.366(3) 4 ?
Cu1 O1 2.366(3) 8 ?
O2 C2 1.247(4) . ?
O1 C1 1.231(5) . ?
O3 C1 1.254(5) . ?
N1 C3 1.449(6) 2 ?
N1 C3 1.449(6) . ?
N1 H3 0.85(4) . ?
N1 H3 0.85(4) 2 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 . 5_666 ?
O2 Cu1 O3 88.28(11) . . ?
O2 Cu1 O3 91.72(11) 5_666 . ?
O2 Cu1 O3 91.72(11) . 5_666 ?
O2 Cu1 O3 88.28(11) 5_666 5_666 ?
O3 Cu1 O3 180.0 . 5_666 ?
O2 Cu1 O1 88.21(11) . 4 ?
O2 Cu1 O1 91.79(11) 5_666 4 ?
O3 Cu1 O1 92.22(13) . 4 ?
O3 Cu1 O1 87.78(13) 5_666 4 ?
O2 Cu1 O1 91.79(11) . 8 ?
O2 Cu1 O1 88.21(11) 5_666 8 ?
O3 Cu1 O1 87.78(13) . 8 ?
O3 Cu1 O1 92.22(13) 5_666 8 ?
O1 Cu1 O1 180.0 4 8 ?
C2 O2 Cu1 122.8(3) . . ?
C1 O1 Cu1 124.3(2) . 4_545 ?
C1 O3 Cu1 124.7(3) . . ?
C3 N1 C3 113.3(6) 2 . ?
C3 N1 H3 112(4) 2 . ?
C3 N1 H3 106(4) . . ?
C3 N1 H3 106(4) 2 2 ?
C3 N1 H3 112(4) . 2 ?
H3 N1 H3 108(7) . 2 ?
O2 C2 O2 123.9(5) . 2_556 ?
O2 C2 H2 118.1 . . ?
O2 C2 H2 118.1 2_556 . ?
O1 C1 O3 124.8(4) . . ?
O1 C1 H1 117.6 . . ?
O3 C1 H1 117.6 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.371
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.082

_shelx_res_file                  
;
TITL DMACuF_c1_p04_s in I2/a
    DMACuF_c1_p04_s.res
    created by SHELXL-2016/6 at 12:16:25 on 27-Sep-2017
REM I2/a (#15 in standard setting)
CELL 0.41108  11.271964   8.529472   8.561078  90.0000  95.1904  90.0000
ZERR    4.00   0.000142   0.000268   0.000251   0.0000   0.0017   0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00
L.S. 10
SIZE 0.06 0.04 0.03
ACTA
BOND $H
LIST 4
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.030800    1.707000
FVAR       2.85221
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01691    0.03319 =
         0.02208   -0.00242   -0.00218    0.00170
O2    4    0.348009    0.611553    0.507576    11.00000    0.02002    0.03588 =
         0.03949   -0.00157   -0.00282    0.00009

O1    4    0.424479    0.225500    0.117823    11.00000    0.03498    0.03905 =
         0.03296   -0.00900   -0.00588    0.00494
O3    4    0.437740    0.413230    0.295151    11.00000    0.03137    0.04456 =
         0.02888   -0.00743   -0.00654    0.00989
N1    3    0.250000    0.439564    0.000000    10.50000    0.02780    0.03475 =
         0.04411    0.00000   -0.00895    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.197086    0.381301   -0.046782    11.00000   -1.20000
C2    1    0.250000    0.542777    0.500000    10.50000    0.01806    0.03298 =
         0.02772    0.00000   -0.00037    0.00000
AFIX  43
H2    2    0.249999    0.433743    0.499999    10.50000   -1.20000
AFIX   0
C1    1    0.468756    0.284657    0.240693    11.00000    0.02359    0.03549 =
         0.03419   -0.00261   -0.00440    0.00183
AFIX  43
H1    2    0.529724    0.229927    0.297314    11.00000   -1.20000
AFIX   0
C3    1    0.189611    0.532927    0.109935    11.00000    0.04624    0.06094 =
         0.04101    0.00466    0.01036    0.00310
AFIX  33
H4    2    0.151454    0.464898    0.179398    11.00000   -1.20000
H5    2    0.246529    0.597872    0.169793    11.00000   -1.20000
H6    2    0.130837    0.597871    0.053454    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_p04_s in I2/a
REM R1 =  0.0359 for     556 Fo > 4sig(Fo)  and  0.0501 for all     736 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0308      1.7068

REM Highest difference peak  0.371,  deepest hole -0.364,  1-sigma level  0.082
Q1    1   0.5106  0.5833  0.5839  11.00000  0.05    0.34
Q2    1   0.4886  0.5701  0.4272  11.00000  0.05    0.33
Q3    1   0.1487  0.3856  0.4881  11.00000  0.05    0.30
Q4    1   0.1792  0.3722  0.3005  11.00000  0.05    0.28
Q5    1   0.4436  0.4900  0.1581  11.00000  0.05    0.28
Q6    1   0.4356  0.5806  0.2969  11.00000  0.05    0.27
Q7    1   0.3662  0.3669  0.2748  11.00000  0.05    0.26
Q8    1   0.2500  0.5677  0.0000  10.50000  0.05    0.25
Q9    1   0.2035  0.3893  0.2098  11.00000  0.05    0.25
Q10   1   0.3823  0.2069  0.1905  11.00000  0.05    0.25
Q11   1   0.5742  0.2739  0.3805  11.00000  0.05    0.25
Q12   1   0.5129  0.6491  0.5131  11.00000  0.05    0.24
Q13   1   0.1423  0.5184  0.0904  11.00000  0.05    0.23
Q14   1   0.4221  0.2716  0.1597  11.00000  0.05    0.23
Q15   1   0.1778  0.5723 -0.0576  11.00000  0.05    0.23
Q16   1  -0.0300  0.5967  0.0204  11.00000  0.05    0.23
Q17   1   0.0867  0.4603  0.0980  11.00000  0.05    0.22
Q18   1   0.3263  0.1877  0.1594  11.00000  0.05    0.22
Q19   1   0.3740  0.2747  0.1233  11.00000  0.05    0.22
Q20   1   0.0565  0.4622  0.2527  11.00000  0.05    0.21
;
_shelx_res_checksum              68840
####################################################################### 
# 
# 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_DMAMnF_c3_p04_s
_database_code_depnum_ccdc_archive 'CCDC 1837768'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1791 0.2616 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.1738(4)
_cell_length_b                   8.1738(4)
_cell_length_c                   21.4104(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1238.81(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    149
_cell_measurement_theta_min      2.7590
_cell_measurement_theta_max      15.8040

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.357
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77371
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '3.36 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            750
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.884
_diffrn_reflns_theta_max         19.597
_diffrn_reflns_theta_full        14.283
_diffrn_measured_fraction_theta_max 0.512
_diffrn_measured_fraction_theta_full 0.855
_diffrn_reflns_Laue_measured_fraction_max 0.512
_diffrn_reflns_Laue_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.512
_diffrn_reflns_point_group_measured_fraction_full 0.855
_reflns_number_total             323
_reflns_number_gt                272
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0420P)²+3.1465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         323
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1137
_refine_ls_wR_factor_gt          0.0982
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_restrained_S_all      1.249
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mn1 Mn 0.666667 0.333333 0.333333 0.0322(4) Uani 1 6 d S T P . .
N1 N 0.7446(15) 0.333333 0.083333 0.048(3) Uani 0.3333 2 d DS T P . .
H3 H 0.774(9) 0.241(6) 0.081(7) 0.058 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0271(3) 0.071(2) Uani 1 3 d DS T P . .
H2 H 0.572(6) 0.187(2) 0.014(2) 0.085 Uiso 1 1 d D U . . .
O1 O 0.8674(3) 0.3039(3) 0.27742(11) 0.0464(6) Uani 1 1 d . . . . .
C1 C 1.000000 0.4411(5) 0.250000 0.0365(8) Uani 1 2 d S T P . .
H1 H 1.000000 0.554918 0.250000 0.044 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0339(5) 0.0339(5) 0.0288(5) 0.000 0.000 0.0170(2)
N1 0.045(4) 0.038(5) 0.059(6) -0.014(7) -0.007(3) 0.019(2)
C2 0.091(4) 0.091(4) 0.031(2) 0.000 0.000 0.0454(18)
O1 0.0453(12) 0.0446(12) 0.0489(11) 0.0055(11) 0.0137(11) 0.0222(10)
C1 0.036(2) 0.0364(14) 0.0372(15) 0.0002(9) 0.0003(17) 0.0180(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
Mn1 O1 2.139(2) 31_655 ?
Mn1 O1 2.140(2) 33_545 ?
Mn1 O1 2.140(2) . ?
Mn1 O1 2.140(2) 3_665 ?
Mn1 O1 2.140(2) 32 ?
Mn1 O1 2.140(2) 2_655 ?
N1 N1 1.10(2) 3_665 ?
N1 N1 1.10(2) 2_655 ?
N1 C2 1.363(7) 16_544 ?
N1 C2 1.363(7) . ?
O1 C1 1.250(3) . ?

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 Mn1 O1 91.74(9) 31_655 33_545 ?
O1 Mn1 O1 180.00(12) 31_655 . ?
O1 Mn1 O1 88.26(9) 33_545 . ?
O1 Mn1 O1 88.26(9) 31_655 3_665 ?
O1 Mn1 O1 180.0 33_545 3_665 ?
O1 Mn1 O1 91.74(9) . 3_665 ?
O1 Mn1 O1 91.74(9) 31_655 32 ?
O1 Mn1 O1 91.74(9) 33_545 32 ?
O1 Mn1 O1 88.26(9) . 32 ?
O1 Mn1 O1 88.26(9) 3_665 32 ?
O1 Mn1 O1 88.26(9) 31_655 2_655 ?
O1 Mn1 O1 88.26(9) 33_545 2_655 ?
O1 Mn1 O1 91.74(9) . 2_655 ?
O1 Mn1 O1 91.74(9) 3_665 2_655 ?
O1 Mn1 O1 180.0 32 2_655 ?
N1 N1 N1 60.000(1) 3_665 2_655 ?
N1 N1 C2 66.1(4) 3_665 16_544 ?
N1 N1 C2 66.1(4) 2_655 16_544 ?
N1 N1 C2 66.1(4) 3_665 . ?
N1 N1 C2 66.1(4) 2_655 . ?
C2 N1 C2 124.3(9) 16_544 . ?
N1 C2 N1 47.7(8) . 3_665 ?
N1 C2 N1 47.7(8) . 2_655 ?
N1 C2 N1 47.7(8) 3_665 2_655 ?
C1 O1 Mn1 122.1(2) . . ?
O1 C1 O1 124.7(4) 6_765 . ?

_refine_diff_density_max         0.328
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.077

_shelx_res_file                  
;
TITL DMAMnF_c3_p04_s in R-3c
    DMAMnF_c3_p04_s.res
    created by SHELXL-2016/6 at 10:30:24 on 23-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41119   8.173822   8.173822  21.410408  90.0000  90.0000 120.0000
ZERR    6.00   0.000404   0.000404   0.000567   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Mn
DISP $C -0.00006  0.00048  5.14212!source kissel
DISP $H -0.00003  0.00000  0.64130!source kissel
DISP $N  0.00062  0.00099  7.19266!source kissel
DISP $O  0.00180  0.00183 10.15895!source kissel
DISP $Mn  0.17908  0.26161 636.31605!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT -1 1 4

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
TEMP 20
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.042000    3.146500
FVAR       3.63169
MOLE   1
MN1   5    0.666667    0.333333    0.333333    10.16667    0.03391    0.03391 =
         0.02883    0.00000    0.00000    0.01696
N1    3    0.744557    0.333333    0.083333    10.16667    0.04457    0.03800 =
         0.05920   -0.01414   -0.00707    0.01900
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.773562    0.241024    0.081301    10.33333   -1.20000
C2    1    0.666667    0.333333    0.027059    10.33333    0.09071    0.09071 =
         0.03075    0.00000    0.00000    0.04536
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.572299    0.186770    0.013799    11.00000   -1.20000
O1    4    0.867400    0.303908    0.277421    11.00000    0.04534    0.04455 =
         0.04888    0.00551    0.01375    0.02217
C1    1    1.000000    0.441140    0.250000    10.50000    0.03594    0.03635 =
         0.03718    0.00017    0.00035    0.01797
AFIX  43
H1    2    1.000000    0.554918    0.250000    10.50000   -1.20000
AFIX   0
HKLF 4




REM  DMAMnF_c3_p04_s in R-3c
REM R1 =  0.0410 for     272 Fo > 4sig(Fo)  and  0.0509 for all     323 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0420      3.1476

REM Highest difference peak  0.328,  deepest hole -0.464,  1-sigma level  0.077
Q1    1   0.6411  0.2865 -0.0084  11.00000  0.05    0.33
Q2    1   0.8617  0.5601  0.2752  11.00000  0.05    0.29
Q3    1   0.5051  0.2256  0.3568  11.00000  0.05    0.27
Q4    1   0.9943  0.5752  0.2825  11.00000  0.05    0.25
Q5    1   0.8191  0.3594  0.3198  11.00000  0.05    0.24
Q6    1   0.6667  0.3333  0.3774  10.33333  0.05    0.24
Q7    1   0.7038  0.2520  0.2518  11.00000  0.05    0.22
Q8    1   0.7643  0.2751  0.3015  11.00000  0.05    0.22
Q9    1   0.6704  0.4533  0.3761  11.00000  0.05    0.21
Q10   1   0.9462  0.3858  0.2966  11.00000  0.05    0.19
Q11   1   1.0861  0.6947  0.2817  11.00000  0.05    0.18
Q12   1   0.7504  0.1628  0.1118  11.00000  0.05    0.18
Q13   1   1.0405  0.5483  0.3216  11.00000  0.05    0.18
Q14   1   0.7777  0.1597  0.3118  11.00000  0.05    0.17
Q15   1   0.5199  0.0390 -0.0261  11.00000  0.05    0.17
Q16   1   1.1014  0.5931  0.2607  11.00000  0.05    0.17
Q17   1   0.8555  0.1903  0.1014  11.00000  0.05    0.16
Q18   1   0.6615  0.2625 -0.0343  11.00000  0.05    0.16
Q19   1   0.7316  0.1848  0.0675  11.00000  0.05    0.16
Q20   1   0.8065  0.3598  0.2581  11.00000  0.05    0.15
;
_shelx_res_checksum              15385

# start Validation Reply Form
_vrf_PLAT029_DMAMnF_c3_p04_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.855 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAMnF_c3_p04_s     
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.82 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAMnF_c3_p04_s     
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.78 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances.  In addition, as the (CH3)2NH2 unit
is dynamically disordered, accurate positioning of the H atoms may not
always be possible.
;
_vrf_PLAT911_DMAMnF_c3_p04_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 35 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMAMnF_c3_p04_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMACuF_c2_p12
_database_code_depnum_ccdc_archive 'CCDC 1837747'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c2_p12       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.551 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT043_DMACuF_c2_p12       
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      11.08 Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT088_DMACuF_c2_p12       
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.08 Note
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired. In addition, there is a reduction in resolution for this pressure point, reducing the number of relections measured compared to the lower pressure points.
;
_vrf_PLAT911_DMACuF_c2_p12       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        299 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_CHEMW03_DMACuF_c2_p12       
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT041_DMACuF_c2_p12       
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT068_DMACuF_c2_p12       
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT148_DMACuF_c2_p12       
;
PROBLEM: s.u. on the      c    - Axis is (Too) Large ....      0.006 Ang.
RESPONSE: The diffraction spots are broader giving rise to larger errors in the unit cell parameters.
;
_vrf_PLAT155_DMACuF_c2_p12       
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The cell was kept in the given setting so as to be more comparable to the ambient phase unit cell.
;
_vrf_PLAT202_DMACuF_c2_p12       
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check
RESPONSE: Due to the many parameters in the refinement, refinement of isotropic thermal parameters were preffered.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4687 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.3448(17)
_cell_length_b                   5.871(2)
_cell_length_c                   5.670(6)
_cell_angle_alpha                96.33(8)
_cell_angle_beta                 88.41(6)
_cell_angle_gamma                96.33(3)
_cell_volume                     175.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    56
_cell_measurement_theta_min      3.6880
_cell_measurement_theta_max      12.6440

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_F_000             125
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.700
_shelx_estimated_absorpt_T_min   0.953
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '8.48 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            426
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.218
_diffrn_reflns_theta_max         14.816
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.543
_diffrn_measured_fraction_theta_full 0.551
_diffrn_reflns_Laue_measured_fraction_max 0.543
_diffrn_reflns_Laue_measured_fraction_full 0.551
_diffrn_reflns_point_group_measured_fraction_max 0.543
_diffrn_reflns_point_group_measured_fraction_full 0.551
_reflns_number_total             426
_reflns_number_gt                285
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1330P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         426
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0746
_refine_ls_wR_factor_ref         0.2022
_refine_ls_wR_factor_gt          0.1838
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0454(12) Uani 1 2 d S . P . .
O1 O 0.645(3) 0.638(4) 0.804(3) 0.043(4) Uiso 0.5 1 d . . P . .
O2 O 0.723(3) 0.579(4) 1.163(3) 0.042(4) Uiso 0.5 1 d . . P . .
O3 O -0.185(3) 0.603(4) 0.346(4) 0.044(4) Uiso 0.5 1 d . . P . .
O4 O 0.222(3) 0.599(4) 0.356(3) 0.040(4) Uiso 0.5 1 d . . P . .
O5 O 0.323(3) -0.181(5) 0.406(4) 0.054(5) Uiso 0.5 1 d . . P . .
O6 O 0.366(3) 0.185(5) 0.388(4) 0.058(5) Uiso 0.5 1 d . . P . .
C1 C 0.593(3) 0.542(5) 0.986(4) 0.032(5) Uiso 0.5 1 d . . P . .
C3 C 0.428(3) 0.004(6) 0.466(4) 0.035(6) Uiso 0.5 1 d . . P . .
C2 C 0.012(3) 0.545(4) 0.431(3) 0.018(4) Uiso 0.5 1 d . . P . .
C4 C 0.175(3) -0.099(5) 0.939(4) 0.081(5) Uiso 1 1 d . . . . .
N1 N -0.002(4) -0.016(6) 1.087(4) 0.045(5) Uiso 0.5 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0396(13) 0.056(3) 0.0346(14) -0.0084(18) -0.0085(8) -0.0095(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
Cu1 O4 1.891(15) . ?
Cu1 O4 1.891(15) 2_666 ?
Cu1 O3 1.940(17) 2_566 ?
Cu1 O3 1.940(17) 1_655 ?
Cu1 O6 1.95(3) 2_666 ?
Cu1 O6 1.95(3) . ?
Cu1 O1 1.961(18) 2_666 ?
Cu1 O1 1.961(18) . ?
Cu1 O2 2.288(19) 1_554 ?
Cu1 O2 2.288(19) 2_667 ?
Cu1 O5 2.31(2) 1_565 ?
Cu1 O5 2.31(2) 2_656 ?
O1 C1 1.24(3) . ?
O1 O6 1.59(3) 2_666 ?
O1 O4 1.78(3) 2_666 ?
O2 O3 1.15(3) 1_656 ?
O2 C1 1.22(3) . ?
O3 C2 1.26(2) . ?
O3 C2 1.92(2) 2_566 ?
O4 C2 1.21(2) . ?
O4 O5 1.35(3) 1_565 ?
O4 C2 1.91(2) 2_566 ?
O5 C3 1.18(4) . ?
O5 C3 1.72(3) 2_656 ?
O6 C3 1.28(4) . ?
O6 C3 1.92(4) 2_656 ?
C1 C1 1.08(4) 2_667 ?
C3 C3 0.88(4) 2_656 ?
C2 C2 0.99(3) 2_566 ?
C4 N1 1.22(3) 2_557 ?
C4 N1 1.34(4) . ?
N1 N1 1.03(4) 2_557 ?

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
O4 Cu1 O4 180.0(4) . 2_666 ?
O4 Cu1 O3 68.7(7) . 2_566 ?
O4 Cu1 O3 111.3(7) 2_666 2_566 ?
O4 Cu1 O3 111.3(7) . 1_655 ?
O4 Cu1 O3 68.7(7) 2_666 1_655 ?
O3 Cu1 O3 180.0 2_566 1_655 ?
O4 Cu1 O6 92.6(9) . 2_666 ?
O4 Cu1 O6 87.4(9) 2_666 2_666 ?
O3 Cu1 O6 113.8(9) 2_566 2_666 ?
O3 Cu1 O6 66.2(9) 1_655 2_666 ?
O4 Cu1 O6 87.4(9) . . ?
O4 Cu1 O6 92.6(9) 2_666 . ?
O3 Cu1 O6 66.2(9) 2_566 . ?
O3 Cu1 O6 113.8(9) 1_655 . ?
O6 Cu1 O6 180.0(9) 2_666 . ?
O4 Cu1 O1 55.1(9) . 2_666 ?
O4 Cu1 O1 124.9(9) 2_666 2_666 ?
O3 Cu1 O1 88.3(7) 2_566 2_666 ?
O3 Cu1 O1 91.7(7) 1_655 2_666 ?
O6 Cu1 O1 132.1(9) 2_666 2_666 ?
O6 Cu1 O1 47.9(9) . 2_666 ?
O4 Cu1 O1 124.9(9) . . ?
O4 Cu1 O1 55.1(9) 2_666 . ?
O3 Cu1 O1 91.7(7) 2_566 . ?
O3 Cu1 O1 88.3(7) 1_655 . ?
O6 Cu1 O1 47.9(9) 2_666 . ?
O6 Cu1 O1 132.1(9) . . ?
O1 Cu1 O1 180.0 2_666 . ?
O4 Cu1 O2 86.3(7) . 1_554 ?
O4 Cu1 O2 93.7(7) 2_666 1_554 ?
O3 Cu1 O2 149.8(6) 2_566 1_554 ?
O3 Cu1 O2 30.2(6) 1_655 1_554 ?
O6 Cu1 O2 82.9(9) 2_666 1_554 ?
O6 Cu1 O2 97.1(9) . 1_554 ?
O1 Cu1 O2 62.9(7) 2_666 1_554 ?
O1 Cu1 O2 117.1(7) . 1_554 ?
O4 Cu1 O2 93.7(7) . 2_667 ?
O4 Cu1 O2 86.3(7) 2_666 2_667 ?
O3 Cu1 O2 30.2(6) 2_566 2_667 ?
O3 Cu1 O2 149.8(6) 1_655 2_667 ?
O6 Cu1 O2 97.1(9) 2_666 2_667 ?
O6 Cu1 O2 82.9(9) . 2_667 ?
O1 Cu1 O2 117.1(7) 2_666 2_667 ?
O1 Cu1 O2 62.9(7) . 2_667 ?
O2 Cu1 O2 180.0(11) 1_554 2_667 ?
O4 Cu1 O5 35.6(8) . 1_565 ?
O4 Cu1 O5 144.4(8) 2_666 1_565 ?
O3 Cu1 O5 89.2(8) 2_566 1_565 ?
O3 Cu1 O5 90.8(8) 1_655 1_565 ?
O6 Cu1 O5 57.3(8) 2_666 1_565 ?
O6 Cu1 O5 122.7(8) . 1_565 ?
O1 Cu1 O5 82.7(9) 2_666 1_565 ?
O1 Cu1 O5 97.3(9) . 1_565 ?
O2 Cu1 O5 78.9(7) 1_554 1_565 ?
O2 Cu1 O5 101.1(7) 2_667 1_565 ?
O4 Cu1 O5 144.4(8) . 2_656 ?
O4 Cu1 O5 35.6(8) 2_666 2_656 ?
O3 Cu1 O5 90.8(8) 2_566 2_656 ?
O3 Cu1 O5 89.2(8) 1_655 2_656 ?
O6 Cu1 O5 122.7(8) 2_666 2_656 ?
O6 Cu1 O5 57.3(8) . 2_656 ?
O1 Cu1 O5 97.3(9) 2_666 2_656 ?
O1 Cu1 O5 82.7(9) . 2_656 ?
O2 Cu1 O5 101.1(7) 1_554 2_656 ?
O2 Cu1 O5 78.9(7) 2_667 2_656 ?
O5 Cu1 O5 180.0 1_565 2_656 ?
C1 O1 O6 159(2) . 2_666 ?
C1 O1 O4 95.7(19) . 2_666 ?
O6 O1 O4 103.8(15) 2_666 2_666 ?
C1 O1 Cu1 119.7(17) . . ?
O6 O1 Cu1 65.7(11) 2_666 . ?
O4 O1 Cu1 60.5(9) 2_666 . ?
O3 O2 C1 170(2) 1_656 . ?
O3 O2 Cu1 58.0(13) 1_656 1_556 ?
C1 O2 Cu1 112.5(14) . 1_556 ?
O2 O3 C2 136(2) 1_454 . ?
O2 O3 C2 144(2) 1_454 2_566 ?
C2 O3 C2 27.3(12) . 2_566 ?
O2 O3 Cu1 91.8(12) 1_454 1_455 ?
C2 O3 Cu1 115.9(14) . 1_455 ?
C2 O3 Cu1 88.6(11) 2_566 1_455 ?
C2 O4 O5 118(2) . 1_565 ?
C2 O4 O1 112(2) . 2_666 ?
O5 O4 O1 129.5(15) 1_565 2_666 ?
C2 O4 Cu1 118.8(15) . . ?
O5 O4 Cu1 89.4(11) 1_565 . ?
O1 O4 Cu1 64.5(8) 2_666 . ?
C2 O4 C2 26.6(13) . 2_566 ?
O5 O4 C2 121.4(18) 1_565 2_566 ?
O1 O4 C2 103.1(13) 2_666 2_566 ?
Cu1 O4 C2 92.3(10) . 2_566 ?
C3 O5 O4 173(3) . 1_545 ?
C3 O5 C3 28(2) . 2_656 ?
O4 O5 C3 145.0(18) 1_545 2_656 ?
C3 O5 Cu1 118.2(18) . 1_545 ?
O4 O5 Cu1 54.9(12) 1_545 1_545 ?
C3 O5 Cu1 90.0(10) 2_656 1_545 ?
C3 O6 O1 155(2) . 2_666 ?
C3 O6 C3 22.4(17) . 2_656 ?
O1 O6 C3 145.6(13) 2_666 2_656 ?
C3 O6 Cu1 125.1(17) . . ?
O1 O6 Cu1 66.4(12) 2_666 . ?
C3 O6 Cu1 104.3(12) 2_656 . ?
C1 C1 O2 114(4) 2_667 . ?
C1 C1 O1 121(3) 2_667 . ?
O2 C1 O1 123(2) . . ?
C3 C3 O5 112(5) 2_656 . ?
C3 C3 O6 124(5) 2_656 . ?
O5 C3 O6 122(2) . . ?
C3 C3 O5 39(4) 2_656 2_656 ?
O5 C3 O5 152(2) . 2_656 ?
O6 C3 O5 85.7(19) . 2_656 ?
C3 C3 O6 34(3) 2_656 2_656 ?
O5 C3 O6 80(2) . 2_656 ?
O6 C3 O6 157.6(17) . 2_656 ?
O5 C3 O6 72.2(11) 2_656 2_656 ?
C2 C2 O4 120(3) 2_566 . ?
C2 C2 O3 117(2) 2_566 . ?
O4 C2 O3 123.4(18) . . ?
C2 C2 O4 33.5(16) 2_566 2_566 ?
O4 C2 O4 153.4(13) . 2_566 ?
O3 C2 O4 83.2(11) . 2_566 ?
C2 C2 O3 36.0(16) 2_566 2_566 ?
O4 C2 O3 83.9(13) . 2_566 ?
O3 C2 O3 152.7(12) . 2_566 ?
O4 C2 O3 69.5(9) 2_566 2_566 ?
N1 C4 N1 46.8(19) 2_557 . ?
N1 N1 C4 73(3) 2_557 2_557 ?
N1 N1 C4 60(3) 2_557 . ?
C4 N1 C4 133.2(19) 2_557 . ?

_refine_diff_density_max         0.911
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.138

_shelx_res_file                  
;
TITL DMACuF_c2_p12_s_twin in P-1
    DMACuF_c2_p12_twins12_reslim0p8_mask1p5_twin1_hklf5.res
    created by SHELXL-2016/6 at 16:42:07 on 21-Mar-2018
REM P-1 (#2 in standard setting)
CELL 0.41108    5.344791  5.871140   5.670034      96.3272   88.4126  96.3268
ZERR    1.00    0.001670  0.002360   0.005763       0.0767   0.0586   0.0298
LATT  1
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.14091!source kissel
DISP $H -0.00003  0.00000  0.64127!source kissel
DISP $N  0.00062  0.00099  7.19030!source kissel
DISP $O  0.00180  0.00183 10.15475!source kissel
DISP $Cu  0.24634  0.46870 1129.00277!source kissel
UNIT 5.00 11.00 1.00 6.00 1.00
OMIT -2 2 0
OMIT 2 -2 0
OMIT 3 6 0
OMIT -3 -6 0
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 50
SIZE 0.07 0.045 0.02
ACTA
BOND
FMAP 2
PLAN 20
MERG 0
WGHT    0.133000
BASF   0.60391
FVAR      28.46259
MOLE   1
CU1   5    0.500000    0.500000    0.500000    10.50000    0.03962    0.05604 =
         0.03458   -0.00836   -0.00849   -0.00951
O1    4    0.644548    0.637926    0.803596    10.50000    0.04341
O2    4    0.722570    0.578606    1.162687    10.50000    0.04199
O3    4   -0.185290    0.603062    0.346426    10.50000    0.04352
O4    4    0.222201    0.599389    0.356037    10.50000    0.03970
O5    4    0.323086   -0.180655    0.405635    10.50000    0.05353
O6    4    0.365583    0.185430    0.387866    10.50000    0.05763
C1    1    0.592717    0.542340    0.985554    10.50000    0.03201
C3    1    0.427735    0.003878    0.465920    10.50000    0.03453
C2    1    0.011623    0.544932    0.431309    10.50000    0.01824
C4    1    0.174591   -0.099160    0.939379    11.00000    0.08150
N1    3   -0.002446   -0.015543    1.087304    10.50000    0.04492
MOLE   2
HKLF 5 1 0 1 0 1 0 0 0 0 1 1 0




REM  DMACuF_c2_p12_s_twin in P-1
REM R1 =  0.0746 for     285 Fo > 4sig(Fo)  and  0.1021 for all     426 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.1336      0.0000

REM Highest difference peak  0.911,  deepest hole -0.925,  1-sigma level  0.138
Q1    1   0.3619  0.5101  0.5182  11.00000  0.05    0.91
Q2    1   0.4958  0.6702  0.5067  11.00000  0.05    0.62
Q3    1   0.1625 -0.0213  0.8427  11.00000  0.05    0.60
Q4    1   0.4754  0.3853  0.5956  11.00000  0.05    0.49
Q5    1  -0.2603  0.6451  0.4782  11.00000  0.05    0.48
Q6    1   0.5412  0.4811  1.2163  11.00000  0.05    0.45
Q7    1   0.1625  0.5209  0.4795  11.00000  0.05    0.40
Q8    1   0.2050 -0.2263  0.9697  11.00000  0.05    0.38
Q9    1   1.0000  0.5000  1.0000  10.50000  0.05    0.37
Q10   1   0.0041  0.8369  0.4890  11.00000  0.05    0.36
Q11   1   0.1751 -0.1863  0.4197  11.00000  0.05    0.34
Q12   1   0.3378  0.0076  0.4323  11.00000  0.05    0.34
Q13   1   0.3235  0.4861  0.3104  11.00000  0.05    0.34
Q14   1  -0.0053  0.6162  0.5389  11.00000  0.05    0.34
Q15   1  -0.2191  0.4265  0.4155  11.00000  0.05    0.33
Q16   1   0.6072  0.8401  0.8316  11.00000  0.05    0.32
Q17   1   0.0071  0.4041  0.3022  11.00000  0.05    0.32
Q18   1  -0.1777  0.3951  0.3128  11.00000  0.05    0.31
Q19   1   0.2384  0.6572  0.2479  11.00000  0.05    0.31
Q20   1   0.1641  0.2154  0.2665  11.00000  0.05    0.31
;
_shelx_res_checksum              3763
####################################################################### 
# 
# 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_DMAMnF_c3_p05_s
_database_code_depnum_ccdc_archive 'CCDC 1837769'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1791 0.2616 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.1373(6)
_cell_length_b                   8.1373(6)
_cell_length_c                   21.1601(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1213.41(19)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    176
_cell_measurement_theta_min      3.3410
_cell_measurement_theta_max      15.3230

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.365
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65009
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '4.37 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            736
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.785
_diffrn_reflns_theta_max         19.670
_diffrn_reflns_theta_full        14.283
_diffrn_measured_fraction_theta_max 0.499
_diffrn_measured_fraction_theta_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.499
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.499
_diffrn_reflns_point_group_measured_fraction_full 0.849
_reflns_number_total             314
_reflns_number_gt                244
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0870P)²+2.8722P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         314
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1643
_refine_ls_wR_factor_gt          0.1437
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mn1 Mn 0.666667 0.333333 0.333333 0.0443(6) Uani 1 6 d S T P . .
N1 N 0.7426(19) 0.333333 0.083333 0.064(4) Uani 0.3333 2 d DS T P . .
H3 H 0.800(12) 0.285(19) 0.107(5) 0.077 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0267(4) 0.090(4) Uani 1 3 d DS T P . .
H2 H 0.579(8) 0.192(4) 0.006(3) 0.107 Uiso 1 1 d D U . . .
O1 O 0.8663(4) 0.3007(4) 0.27695(14) 0.0607(9) Uani 1 1 d . . . . .
C1 C 1.000000 0.4385(7) 0.250000 0.0490(11) Uani 1 2 d S T P . .
H1 H 0.999997 0.552837 0.249999 0.059 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0486(7) 0.0486(7) 0.0359(7) 0.000 0.000 0.0243(3)
N1 0.056(6) 0.069(8) 0.071(9) -0.019(11) -0.010(5) 0.035(4)
C2 0.116(6) 0.116(6) 0.036(3) 0.000 0.000 0.058(3)
O1 0.0607(18) 0.0611(17) 0.0593(14) 0.0089(14) 0.0184(14) 0.0297(14)
C1 0.051(3) 0.0505(19) 0.046(2) -0.0022(11) -0.004(2) 0.0257(14)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.136(3) 31_655 ?
Mn1 O1 2.136(3) 33_545 ?
Mn1 O1 2.136(3) . ?
Mn1 O1 2.136(3) 3_665 ?
Mn1 O1 2.136(3) 32 ?
Mn1 O1 2.136(3) 2_655 ?
N1 N1 1.07(3) 3_665 ?
N1 N1 1.07(3) 2_655 ?
N1 C2 1.348(9) 16_544 ?
N1 C2 1.348(9) . ?
O1 C1 1.244(4) . ?

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 Mn1 O1 91.84(11) 31_655 33_545 ?
O1 Mn1 O1 180.0 31_655 . ?
O1 Mn1 O1 88.16(11) 33_545 . ?
O1 Mn1 O1 88.16(11) 31_655 3_665 ?
O1 Mn1 O1 180.0 33_545 3_665 ?
O1 Mn1 O1 91.84(11) . 3_665 ?
O1 Mn1 O1 91.84(11) 31_655 32 ?
O1 Mn1 O1 91.84(11) 33_545 32 ?
O1 Mn1 O1 88.16(11) . 32 ?
O1 Mn1 O1 88.16(11) 3_665 32 ?
O1 Mn1 O1 88.16(11) 31_655 2_655 ?
O1 Mn1 O1 88.16(11) 33_545 2_655 ?
O1 Mn1 O1 91.84(11) . 2_655 ?
O1 Mn1 O1 91.84(11) 3_665 2_655 ?
O1 Mn1 O1 180.0 32 2_655 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 66.6(5) 3_665 16_544 ?
N1 N1 C2 66.6(5) 2_655 16_544 ?
N1 N1 C2 66.6(5) 3_665 . ?
N1 N1 C2 66.6(5) 2_655 . ?
C2 N1 C2 125.5(12) 16_544 . ?
N1 C2 N1 46.7(10) . 3_665 ?
N1 C2 N1 46.7(10) . 2_655 ?
N1 C2 N1 46.7(10) 3_665 2_655 ?
C1 O1 Mn1 121.4(3) . . ?
O1 C1 O1 124.6(5) 6_765 . ?

_refine_diff_density_max         0.421
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.089

_shelx_res_file                  
;
TITL DMAMnF_c3_p05_s in R-3c
    DMAMnF_c3_p05_s.res
    created by SHELXL-2016/6 at 11:45:02 on 17-Apr-2018
REM R-3c (#167 in standard setting)
CELL 0.41119   8.137300   8.137300  21.160061  90.0000  90.0000 120.0000
ZERR    6.00   0.000630   0.000630   0.000722   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Mn
DISP $C -0.00006  0.00048  5.14212!source kissel
DISP $H -0.00003  0.00000  0.64130!source kissel
DISP $N  0.00062  0.00099  7.19266!source kissel
DISP $O  0.00180  0.00183 10.15895!source kissel
DISP $Mn  0.17908  0.26161 636.31605!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 1 -2 6
OMIT -5 12 4
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
TEMP 20
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.087000    2.872200
FVAR       3.73069
MOLE   1
MN1   5    0.666667    0.333333    0.333333    10.16667    0.04856    0.04856 =
         0.03585    0.00000    0.00000    0.02428
N1    3    0.742557    0.333333    0.083333    10.16667    0.05591    0.06947 =
         0.07070   -0.01908   -0.00954    0.03473
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.799839    0.284568    0.106971    10.33333   -1.20000
C2    1    0.666667    0.333333    0.026690    10.33333    0.11648    0.11648 =
         0.03557    0.00000    0.00000    0.05824
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.579036    0.191623    0.006391    11.00000   -1.20000
O1    4    0.866267    0.300684    0.276949    11.00000    0.06065    0.06109 =
         0.05926    0.00885    0.01844    0.02967
C1    1    1.000000    0.438549    0.250000    10.50000    0.05141    0.05046 =
         0.04557   -0.00221   -0.00442    0.02570
AFIX  43
H1    2    0.999997    0.552837    0.249999    10.50000   -1.20000
AFIX   0
HKLF 4




REM  DMAMnF_c3_p05_s in R-3c
REM R1 =  0.0532 for     244 Fo > 4sig(Fo)  and  0.0643 for all     314 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0867      2.8913

REM Highest difference peak  0.421,  deepest hole -0.539,  1-sigma level  0.089
Q1    1   0.8683  0.5616  0.2773  11.00000  0.05    0.42
Q2    1   0.7994  0.3267  0.3086  11.00000  0.05    0.33
Q3    1   0.5000  0.0000  0.0000  10.50000  0.05    0.27
Q4    1   1.0000  0.6822  0.2500  10.50000  0.05    0.26
Q5    1   0.9080  0.2349  0.1469  11.00000  0.05    0.24
Q6    1   0.5312  0.2570  0.0152  11.00000  0.05    0.21
Q7    1   0.9992  0.5826  0.2832  11.00000  0.05    0.21
Q8    1   0.6667  0.3333  0.3807  10.33333  0.05    0.20
Q9    1   0.7581  0.2151  0.0751  11.00000  0.05    0.20
Q10   1   1.0238  0.5048  0.3006  11.00000  0.05    0.18
Q11   1   0.6667  0.3333 -0.0197  10.33333  0.05    0.18
Q12   1   1.0821  0.6482  0.2876  11.00000  0.05    0.18
Q13   1   0.6016  0.0276  0.0185  11.00000  0.05    0.17
Q14   1   0.7208  0.2685  0.2506  11.00000  0.05    0.17
Q15   1   0.9684  0.3815  0.3001  11.00000  0.05    0.16
Q16   1   0.5249  0.1904  0.3556  11.00000  0.05    0.15
Q17   1   0.4769  0.2148 -0.0328  11.00000  0.05    0.15
Q18   1   0.9945  0.3190  0.3055  11.00000  0.05    0.15
Q19   1   0.7309  0.1355  0.3154  11.00000  0.05    0.14
Q20   1   1.0000  0.2973  0.2500  10.50000  0.05    0.14
;
_shelx_res_checksum              9468




# start Validation Reply Form
_vrf_PLAT029_DMAMnF_c3_p05_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.849 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAMnF_c3_p05_s     
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.78 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAMnF_c3_p05_s     
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.31 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAMnF_c3_p05_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 37 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT088_DMAMnF_c3_p05_s     
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.81 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. Additionally,
the positioning of the hydrogen atoms for the dynamically disordered 
(CH3)2NH2 unit could not be performed with standard AFIX commands. Instead
distance restraints are used which increases the number of parameters as the
hydrogen positions are refined.
;
_vrf_PLAT978_DMAMnF_c3_p05_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
# end Validation Reply Form

#==============================================================================
####################################################################### 
# 
# 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_DMACuF_c1_p05_s
_database_code_depnum_ccdc_archive 'CCDC 1837740'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c1_p05_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.598 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c1_p05_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        292 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT905_DMACuF_c1_p05_s     
;
PROBLEM: Negative K value in the Analysis of Variance ...     -0.437 Report
RESPONSE: The negative K value is only observed at the highest resolution of 0.58 Angstrom where the weakest reflections are observed.
;
_vrf_PLAT978_DMACuF_c1_p05_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.22268(13)
_cell_length_b                   8.4953(3)
_cell_length_c                   8.4836(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.9859(18)
_cell_angle_gamma                90
_cell_volume                     805.77(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    246
_cell_measurement_theta_min      2.9680
_cell_measurement_theta_max      17.3460

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.610
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         '2.40 GPa'
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1212
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.741
_diffrn_reflns_theta_max         20.794
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.334
_diffrn_measured_fraction_theta_full 0.598
_diffrn_reflns_Laue_measured_fraction_max 0.334
_diffrn_reflns_Laue_measured_fraction_full 0.598
_diffrn_reflns_point_group_measured_fraction_max 0.334
_diffrn_reflns_point_group_measured_fraction_full 0.598
_reflns_number_total             729
_reflns_number_gt                535
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0297P)²+3.0001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         729
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0259(2) Uani 1 2 d S . P . .
O2 O 0.3484(2) 0.6133(4) 0.5076(4) 0.0327(7) Uani 1 1 d . . . . .
O1 O 0.4233(3) 0.2245(4) 0.1168(4) 0.0371(8) Uani 1 1 d . . . . .
O3 O 0.4376(3) 0.4142(5) 0.2932(4) 0.0364(8) Uani 1 1 d . . . . .
N1 N 0.250000 0.4407(9) 0.000000 0.0405(14) Uani 1 2 d DS T P . .
H3 H 0.196(5) 0.371(7) -0.055(8) 0.049 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5439(8) 0.500000 0.0287(12) Uani 1 2 d S T P . .
H2 H 0.250001 0.434389 0.500003 0.034 Uiso 1 2 calc R U P . .
C1 C 0.4677(4) 0.2845(6) 0.2410(6) 0.0329(10) Uani 1 1 d . . . . .
H1 H 0.527798 0.228968 0.299460 0.039 Uiso 1 1 calc R U . . .
C3 C 0.1887(5) 0.5334(7) 0.1102(7) 0.0494(14) Uani 1 1 d . . . . .
H4 H 0.150003 0.464712 0.179784 0.059 Uiso 1 1 calc R U . . .
H5 H 0.245343 0.598612 0.171223 0.059 Uiso 1 1 calc R U . . .
H6 H 0.129875 0.598608 0.053109 0.059 Uiso 1 1 calc R U . . .

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
Cu1 0.0183(3) 0.0354(6) 0.0234(6) -0.0019(2) -0.0018(3) 0.0013(2)
O2 0.0213(10) 0.038(2) 0.038(2) -0.0015(12) -0.0012(12) 0.0019(11)
O1 0.0348(14) 0.042(3) 0.034(3) -0.0071(13) -0.0041(14) 0.0055(14)
O3 0.0331(13) 0.048(3) 0.027(3) -0.0067(13) -0.0057(14) 0.0081(14)
N1 0.033(2) 0.044(5) 0.042(5) 0.000 -0.005(3) 0.000
C2 0.0191(18) 0.035(4) 0.031(4) 0.000 0.000(2) 0.000
C1 0.0251(15) 0.041(3) 0.032(3) -0.0015(16) -0.0034(17) 0.0009(17)
C3 0.048(3) 0.063(5) 0.039(5) 0.004(2) 0.013(3) 0.000(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
Cu1 O2 1.960(3) 5_666 ?
Cu1 O2 1.960(3) . ?
Cu1 O3 1.971(3) 5_666 ?
Cu1 O3 1.971(3) . ?
Cu1 O1 2.347(3) 4 ?
Cu1 O1 2.347(3) 8 ?
O2 C2 1.249(4) . ?
O1 C1 1.236(6) . ?
O3 C1 1.245(6) . ?
N1 C3 1.442(7) 2 ?
N1 C3 1.442(7) . ?
N1 H3 0.94(5) . ?
N1 H3 0.94(5) 2 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 5_666 . ?
O2 Cu1 O3 88.22(13) 5_666 5_666 ?
O2 Cu1 O3 91.78(13) . 5_666 ?
O2 Cu1 O3 91.78(13) 5_666 . ?
O2 Cu1 O3 88.22(13) . . ?
O3 Cu1 O3 180.0 5_666 . ?
O2 Cu1 O1 91.94(13) 5_666 4 ?
O2 Cu1 O1 88.06(13) . 4 ?
O3 Cu1 O1 87.71(15) 5_666 4 ?
O3 Cu1 O1 92.28(15) . 4 ?
O2 Cu1 O1 88.06(13) 5_666 8 ?
O2 Cu1 O1 91.94(13) . 8 ?
O3 Cu1 O1 92.29(15) 5_666 8 ?
O3 Cu1 O1 87.72(15) . 8 ?
O1 Cu1 O1 180.0 4 8 ?
C2 O2 Cu1 122.2(4) . . ?
C1 O1 Cu1 124.0(3) . 4_545 ?
C1 O3 Cu1 123.9(3) . . ?
C3 N1 C3 113.8(7) 2 . ?
C3 N1 H3 110(4) 2 . ?
C3 N1 H3 110(4) . . ?
C3 N1 H3 110(4) 2 2 ?
C3 N1 H3 110(4) . 2 ?
H3 N1 H3 102(8) . 2 ?
O2 C2 O2 123.7(6) 2_556 . ?
O2 C2 H2 118.2 2_556 . ?
O2 C2 H2 118.2 . . ?
O1 C1 O3 124.5(4) . . ?
O1 C1 H1 117.8 . . ?
O3 C1 H1 117.8 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.549
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.090

_shelx_res_file                  
;
TITL DMACuF_c1_p05_s in I2/a
    DMACuF_c1_p05_s.res
    created by SHELXL-2016/6 at 12:17:13 on 27-Sep-2017
REM I2/a (#15 in standard setting)
CELL 0.41108  11.222682   8.495310   8.483584  90.0000  94.9859  90.0000
ZERR    4.00   0.000129   0.000250   0.000238   0.0000   0.0018   0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00
L.S. 10
SIZE 0.06 0.04 0.03
ACTA
BOND $H
LIST 5
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.029700    3.000100
FVAR       2.83398
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01834    0.03541 =
         0.02341   -0.00191   -0.00183    0.00131
O2    4    0.348435    0.613270    0.507626    11.00000    0.02132    0.03841 =
         0.03771   -0.00153   -0.00120    0.00190

O1    4    0.423303    0.224549    0.116778    11.00000    0.03479    0.04177 =
         0.03351   -0.00705   -0.00414    0.00552
O3    4    0.437640    0.414162    0.293202    11.00000    0.03310    0.04765 =
         0.02694   -0.00665   -0.00573    0.00813
N1    3    0.250000    0.440739    0.000000    10.50000    0.03333    0.04437 =
         0.04243    0.00000   -0.00520    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.196046    0.370995   -0.055317    11.00000   -1.20000
C2    1    0.250000    0.543861    0.500000    10.50000    0.01913    0.03529 =
         0.03131    0.00000    0.00044    0.00000
AFIX  43
H2    2    0.250001    0.434389    0.500003    10.50000   -1.20000
AFIX   0
C1    1    0.467742    0.284516    0.240987    11.00000    0.02507    0.04077 =
         0.03174   -0.00152   -0.00336    0.00089
AFIX  43
H1    2    0.527798    0.228968    0.299460    11.00000   -1.20000
AFIX   0
C3    1    0.188679    0.533415    0.110245    11.00000    0.04811    0.06293 =
         0.03876    0.00373    0.01297   -0.00001
AFIX  33
H4    2    0.150003    0.464712    0.179784    11.00000   -1.20000
H5    2    0.245343    0.598612    0.171223    11.00000   -1.20000
H6    2    0.129875    0.598608    0.053109    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_p05_s in I2/a
REM R1 =  0.0401 for     535 Fo > 4sig(Fo)  and  0.0569 for all     729 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0297      2.9968

REM Highest difference peak  0.549,  deepest hole -0.379,  1-sigma level  0.090
Q1    1   0.5125  0.5798  0.5887  11.00000  0.05    0.55
Q2    1   0.5058  0.4316  0.5773  11.00000  0.05    0.52
Q3    1   0.2500  0.5660  0.0000  10.50000  0.05    0.39
Q4    1   0.4388  0.5798  0.2974  11.00000  0.05    0.38
Q5    1   0.5718  0.5049  0.5657  11.00000  0.05    0.35
Q6    1   0.5778  0.2738  0.3875  11.00000  0.05    0.34
Q7    1   0.1486  0.3871  0.4853  11.00000  0.05    0.33
Q8    1   0.4979  0.3728  0.3555  11.00000  0.05    0.29
Q9    1   0.1803  0.5527 -0.0688  11.00000  0.05    0.29
Q10   1   0.4252  0.5709  0.5225  11.00000  0.05    0.29
Q11   1   0.5025  0.1434  0.1355  11.00000  0.05    0.29
Q12   1   0.4810  0.4815  0.3425  11.00000  0.05    0.28
Q13   1   0.3605  0.5755  0.4256  11.00000  0.05    0.27
Q14   1   0.4501  0.3468  0.0953  11.00000  0.05    0.26
Q15   1   0.2763  0.4419  0.4102  11.00000  0.05    0.26
Q16   1   0.4222  0.2599  0.0051  11.00000  0.05    0.25
Q17   1   0.3529  0.5757  0.5576  11.00000  0.05    0.25
Q18   1   0.5281  0.3457  0.5055  11.00000  0.05    0.25
Q19   1   0.3652  0.3869  0.2780  11.00000  0.05    0.24
Q20   1   0.3520  0.4842  0.3390  11.00000  0.05    0.24
;
_shelx_res_checksum              62292
####################################################################### 
# 
# 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_DMACuF_c1_p07
_database_code_depnum_ccdc_archive 'CCDC 1837742'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c1_p07       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.607 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c1_p07       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        276 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT414_DMACuF_c1_p07       
;
PROBLEM: Short Intra D-H..H-X       H3       ..H6               1.98 Ang.
RESPONSE: The H3 atom forms part of the NH2 group and the H6 is part of the CH3 goup of the dimethylammonium cation. Upon application of pressure, intermolecular and intramolecular contacts can become closer than expected for ambient pressure structures.
;
_vrf_PLAT978_DMACuF_c1_p07       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.08603(18)
_cell_length_b                   8.4489(4)
_cell_length_c                   8.2715(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.553(3)
_cell_angle_gamma                90
_cell_volume                     772.30(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    228
_cell_measurement_theta_min      3.0040
_cell_measurement_theta_max      17.5570

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.104
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.636
_shelx_estimated_absorpt_T_min   0.963
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97883
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         '4.04 GPa'
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1146
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.755
_diffrn_reflns_theta_max         21.050
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.318
_diffrn_measured_fraction_theta_full 0.607
_diffrn_reflns_Laue_measured_fraction_max 0.318
_diffrn_reflns_Laue_measured_fraction_full 0.607
_diffrn_reflns_point_group_measured_fraction_max 0.318
_diffrn_reflns_point_group_measured_fraction_full 0.607
_reflns_number_total             690
_reflns_number_gt                488
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0621P)²+4.0846P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         690
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1499
_refine_ls_wR_factor_gt          0.1259
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0307(3) Uani 1 2 d S . P . .
O2 O 0.3494(3) 0.6190(5) 0.5085(6) 0.0397(10) Uani 1 1 d . . . . .
O1 O 0.4193(4) 0.2190(6) 0.1128(6) 0.0431(11) Uani 1 1 d . . . . .
O3 O 0.4362(3) 0.4157(6) 0.2891(5) 0.0402(10) Uani 1 1 d . . . . .
N1 N 0.250000 0.4436(12) 0.000000 0.050(2) Uani 1 2 d DS T P . .
H3 H 0.181(6) 0.402(10) -0.053(10) 0.060 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5484(11) 0.500000 0.0355(17) Uani 1 2 d S T P . .
H2 H 0.250001 0.438343 0.500000 0.043 Uiso 1 2 calc R U P . .
C1 C 0.4655(5) 0.2830(8) 0.2386(8) 0.0386(13) Uani 1 1 d . . . . .
H1 H 0.526039 0.227993 0.299227 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1867(7) 0.5345(10) 0.1083(11) 0.062(2) Uani 1 1 d . . . . .
H4 H 0.145917 0.465320 0.178210 0.074 Uiso 1 1 calc R U . . .
H5 H 0.242722 0.600043 0.172519 0.074 Uiso 1 1 calc R U . . .
H6 H 0.128399 0.600043 0.048145 0.074 Uiso 1 1 calc R U . . .

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
Cu1 0.0217(4) 0.0446(8) 0.0252(7) -0.0019(3) -0.0017(4) 0.0011(3)
O2 0.0239(13) 0.050(3) 0.045(3) -0.0005(17) 0.0024(16) 0.0009(16)
O1 0.0387(18) 0.054(3) 0.035(3) -0.0059(17) -0.0036(19) 0.0051(19)
O3 0.0340(17) 0.054(3) 0.031(3) -0.0053(16) -0.0034(17) 0.0059(18)
N1 0.038(3) 0.063(7) 0.048(7) 0.000 -0.008(4) 0.000
C2 0.024(2) 0.057(6) 0.025(6) 0.000 0.000(3) 0.000
C1 0.0281(19) 0.052(4) 0.035(4) 0.003(2) -0.002(2) -0.002(2)
C3 0.053(4) 0.089(7) 0.045(7) 0.012(3) 0.010(4) -0.006(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
Cu1 O2 1.954(4) 5_666 ?
Cu1 O2 1.954(4) . ?
Cu1 O3 1.964(4) 5_666 ?
Cu1 O3 1.964(4) . ?
Cu1 O1 2.286(5) 4 ?
Cu1 O1 2.286(5) 8 ?
O2 C2 1.250(6) . ?
O1 C1 1.246(7) . ?
O3 C1 1.248(8) . ?
N1 C3 1.409(10) . ?
N1 C3 1.409(10) 2 ?
N1 H3 0.92(6) . ?
N1 H3 0.92(6) 2 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0(3) 5_666 . ?
O2 Cu1 O3 88.30(18) 5_666 5_666 ?
O2 Cu1 O3 91.70(18) . 5_666 ?
O2 Cu1 O3 91.70(18) 5_666 . ?
O2 Cu1 O3 88.30(18) . . ?
O3 Cu1 O3 180.0 5_666 . ?
O2 Cu1 O1 92.20(17) 5_666 4 ?
O2 Cu1 O1 87.80(17) . 4 ?
O3 Cu1 O1 86.80(19) 5_666 4 ?
O3 Cu1 O1 93.20(19) . 4 ?
O2 Cu1 O1 87.80(17) 5_666 8 ?
O2 Cu1 O1 92.20(17) . 8 ?
O3 Cu1 O1 93.20(19) 5_666 8 ?
O3 Cu1 O1 86.80(19) . 8 ?
O1 Cu1 O1 180.0 4 8 ?
C2 O2 Cu1 120.3(5) . . ?
C1 O1 Cu1 123.0(4) . 4_545 ?
C1 O3 Cu1 122.6(4) . . ?
C3 N1 C3 113.9(10) . 2 ?
C3 N1 H3 94(5) . . ?
C3 N1 H3 110(6) 2 . ?
C3 N1 H3 110(6) . 2 ?
C3 N1 H3 94(5) 2 2 ?
H3 N1 H3 135(10) . 2 ?
O2 C2 O2 123.1(9) . 2_556 ?
O2 C2 H2 118.5 . . ?
O2 C2 H2 118.5 2_556 . ?
O1 C1 O3 124.7(5) . . ?
O1 C1 H1 117.7 . . ?
O3 C1 H1 117.7 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.104

_shelx_res_file                  
;
TITL DMACuF_c1_p07_s_nosg in I2/a
    DMACuF_c1_p07_s_nosg.res
    created by SHELXL-2016/6 at 12:19:08 on 27-Sep-2017
REM I2/a (#15 in standard setting)
CELL 0.41108  11.086028   8.448851   8.271550    90.0000    94.5534    90.0000
ZERR    4.00   0.000183   0.000357   0.000314     0.0000     0.0025     0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00
SIZE 0.06 0.04 0.03
L.S. 10
ACTA
BOND $H
LIST 4
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.062100    4.084600
FVAR       2.81703
CU1   5    0.500000    0.500000    0.500000    10.50000    0.02168    0.04460 =
         0.02521   -0.00190   -0.00168    0.00106
O2    4    0.349440    0.618952    0.508517    11.00000    0.02395    0.04998 =
         0.04508   -0.00047    0.00237    0.00087

O1    4    0.419290    0.219007    0.112833    11.00000    0.03871    0.05419 =
         0.03547   -0.00590   -0.00359    0.00507
O3    4    0.436230    0.415684    0.289061    11.00000    0.03397    0.05434 =
         0.03138   -0.00526   -0.00342    0.00588
N1    3    0.250000    0.443607    0.000000    10.50000    0.03773    0.06258 =
         0.04785    0.00000   -0.00795    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.180857    0.401542   -0.053412    11.00000   -1.20000
C2    1    0.250000    0.548417    0.500000    10.50000    0.02396    0.05692 =
         0.02523    0.00000   -0.00017    0.00000
AFIX  43
H2    2    0.250001    0.438343    0.500000    10.50000   -1.20000
AFIX   0
C1    1    0.465467    0.283016    0.238619    11.00000    0.02813    0.05175 =
         0.03526    0.00299   -0.00242   -0.00181
AFIX  43
H1    2    0.526039    0.227993    0.299227    11.00000   -1.20000
AFIX   0
C3    1    0.186719    0.534492    0.108348    11.00000    0.05251    0.08921 =
         0.04498    0.01153    0.00995   -0.00578
AFIX  33
H4    2    0.145917    0.465320    0.178210    11.00000   -1.20000
H5    2    0.242722    0.600043    0.172519    11.00000   -1.20000
H6    2    0.128399    0.600043    0.048145    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_p07_s_nosg in I2/a
REM R1 =  0.0514 for     488 Fo > 4sig(Fo)  and  0.0734 for all     690 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0622      4.0330

REM Highest difference peak  0.664,  deepest hole -0.427,  1-sigma level  0.104
Q1    1   0.5067  0.5910  0.5864  11.00000  0.05    0.66
Q2    1   0.5029  0.4213  0.5872  11.00000  0.05    0.64
Q3    1   0.1479  0.3771  0.4945  11.00000  0.05    0.52
Q4    1   0.5809  0.2820  0.3752  11.00000  0.05    0.48
Q5    1   0.5384  0.2231  0.2528  11.00000  0.05    0.47
Q6    1   0.5827  0.5040  0.5908  11.00000  0.05    0.46
Q7    1   0.2500  0.5668  0.0000  10.50000  0.05    0.43
Q8    1   0.4394  0.5789  0.2881  11.00000  0.05    0.43
Q9    1   0.5044  0.3394  0.4996  11.00000  0.05    0.41
Q10   1   0.5337  0.1619  0.1451  11.00000  0.05    0.36
Q11   1   0.4766  0.4874  0.3323  11.00000  0.05    0.33
Q12   1   0.2503  0.4964  0.2041  11.00000  0.05    0.33
Q13   1   0.3414  0.7073  0.5753  11.00000  0.05    0.32
Q14   1   0.4776  0.3403  0.3543  11.00000  0.05    0.29
Q15   1   0.3185  0.4433  0.3735  11.00000  0.05    0.29
Q16   1   0.3744  0.4986  0.3517  11.00000  0.05    0.29
Q17   1   0.1371  0.4516  0.3113  11.00000  0.05    0.29
Q18   1   0.4444  0.2020  0.1656  11.00000  0.05    0.28
Q19   1   0.4224  0.5005  0.2137  11.00000  0.05    0.28
Q20   1   0.3178  0.5042  0.4534  11.00000  0.05    0.27
;
_shelx_res_checksum              70583
####################################################################### 
# 
# 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_DMAFeF_c1_s
_database_code_depnum_ccdc_archive 'CCDC 1837754'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.25785(19)
_cell_length_b                   8.25785(19)
_cell_length_c                   22.5102(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1329.37(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    251
_cell_measurement_theta_min      1.9510
_cell_measurement_theta_max      16.0520

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.379
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85251
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '0 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.4109
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            853
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.951
_diffrn_reflns_theta_max         19.321
_diffrn_reflns_theta_full        14.273
_diffrn_measured_fraction_theta_max 0.505
_diffrn_measured_fraction_theta_full 0.785
_diffrn_reflns_Laue_measured_fraction_max 0.505
_diffrn_reflns_Laue_measured_fraction_full 0.785
_diffrn_reflns_point_group_measured_fraction_max 0.505
_diffrn_reflns_point_group_measured_fraction_full 0.785
_reflns_number_total             331
_reflns_number_gt                267
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0549P)²+4.1239P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         331
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.1239
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.202
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0235(4) Uani 1 6 d S T P . .
N1 N 0.7548(17) 0.333333 0.083333 0.052(4) Uani 0.3333 2 d DS T P . .
H3 H 0.786(9) 0.244(7) 0.081(8) 0.062 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0297(4) 0.065(2) Uani 1 3 d DS T P . .
H2 H 0.575(6) 0.205(4) 0.0056(19) 0.078 Uiso 1 1 d D U . . .
O1 O 0.8753(3) 0.3247(3) 0.27909(11) 0.0388(6) Uani 1 1 d . . . . .
C1 C 1.000000 0.4552(6) 0.250000 0.0354(9) Uani 1 2 d S T P . .
H1 H 0.999998 0.567786 0.250000 0.042 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0208(4) 0.0208(4) 0.0290(6) 0.000 0.000 0.0104(2)
N1 0.035(5) 0.034(6) 0.086(12) -0.018(8) -0.009(4) 0.017(3)
C2 0.074(4) 0.074(4) 0.047(5) 0.000 0.000 0.037(2)
O1 0.0344(12) 0.0342(12) 0.0484(14) 0.0074(10) 0.0129(10) 0.0177(10)
C1 0.031(2) 0.0301(15) 0.046(2) 0.0021(9) 0.0043(18) 0.0153(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
Fe1 O1 2.142(2) 3_665 ?
Fe1 O1 2.142(2) 2_655 ?
Fe1 O1 2.142(2) 31_655 ?
Fe1 O1 2.142(2) . ?
Fe1 O1 2.142(2) 33_545 ?
Fe1 O1 2.142(2) 32 ?
N1 N1 1.26(2) 3_665 ?
N1 N1 1.26(2) 2_655 ?
N1 C2 1.410(11) 16_544 ?
N1 C2 1.410(11) . ?
O1 C1 1.241(3) . ?

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 Fe1 O1 90.71(9) 3_665 2_655 ?
O1 Fe1 O1 89.29(9) 3_665 31_655 ?
O1 Fe1 O1 89.29(9) 2_655 31_655 ?
O1 Fe1 O1 90.71(9) 3_665 . ?
O1 Fe1 O1 90.71(9) 2_655 . ?
O1 Fe1 O1 180.0 31_655 . ?
O1 Fe1 O1 180.0 3_665 33_545 ?
O1 Fe1 O1 89.29(9) 2_655 33_545 ?
O1 Fe1 O1 90.72(9) 31_655 33_545 ?
O1 Fe1 O1 89.28(9) . 33_545 ?
O1 Fe1 O1 89.29(9) 3_665 32 ?
O1 Fe1 O1 180.0 2_655 32 ?
O1 Fe1 O1 90.72(9) 31_655 32 ?
O1 Fe1 O1 89.28(9) . 32 ?
O1 Fe1 O1 90.72(9) 33_545 32 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 63.4(4) 3_665 16_544 ?
N1 N1 C2 63.5(4) 2_655 16_544 ?
N1 N1 C2 63.5(4) 3_665 . ?
N1 N1 C2 63.5(4) 2_655 . ?
C2 N1 C2 117.9(10) 16_544 . ?
N1 C2 N1 53.1(9) . 3_665 ?
N1 C2 N1 53.1(9) . 2_655 ?
N1 C2 N1 53.1(9) 3_665 2_655 ?
C1 O1 Fe1 127.2(2) . . ?
O1 C1 O1 126.1(4) . 6_765 ?

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.086

_shelx_res_file                  
;
TITL DMAFeF_c1_s in R-3c
    DMAFeF_c1_s.res
    created by SHELXL-2016/6 at 17:59:41 on 21-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41090   8.257855   8.257855  22.510208  90.0000  90.0000 120.0000
ZERR    6.00   0.000190   0.000190   0.000565   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT -1 2 0
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.054900    4.123899
FVAR       2.61390
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.02081    0.02081 =
         0.02896    0.00000    0.00000    0.01041
N1    3    0.754783    0.333333    0.083333    10.16667    0.03484    0.03351 =
         0.08619   -0.01805   -0.00903    0.01675
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.785834    0.243629    0.081023    10.33333   -1.20000
C2    1    0.666667    0.333333    0.029684    10.33333    0.07410    0.07410 =
         0.04696    0.00000    0.00000    0.03705
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.574733    0.204572    0.005557    11.00000   -1.20000
O1    4    0.875294    0.324707    0.279091    11.00000    0.03437    0.03418 =
         0.04844    0.00744    0.01290    0.01766
C1    1    1.000000    0.455166    0.250000    10.50000    0.03069    0.03008 =
         0.04561    0.00215    0.00430    0.01535
AFIX  43
H1    2    0.999998    0.567786    0.250000    10.50000   -1.20000
AFIX   0
HKLF 4




REM  DMAFeF_c1_s in R-3c
REM R1 =  0.0394 for     267 Fo > 4sig(Fo)  and  0.0498 for all     331 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0549      4.1263

REM Highest difference peak  0.406,  deepest hole -0.443,  1-sigma level  0.086
Q1    1   0.7169  0.4614  0.3665  11.00000  0.05    0.41
Q2    1   0.8844  0.5495  0.2776  11.00000  0.05    0.27
Q3    1   0.7141  0.2453  0.2331  11.00000  0.05    0.24
Q4    1   0.6667  0.3333 -0.0039  10.33333  0.05    0.23
Q5    1   0.5709  0.1921  0.3526  11.00000  0.05    0.23
Q6    1   0.7153  0.1903  0.0732  11.00000  0.05    0.21
Q7    1   0.7777  0.1774  0.2501  11.00000  0.05    0.21
Q8    1   0.8949  0.3333  0.0833  10.50000  0.05    0.21
Q9    1   0.8897  0.2043  0.3121  11.00000  0.05    0.19
Q10   1   0.4049  0.0590  0.0011  11.00000  0.05    0.19
Q11   1   0.7585  0.3013  0.0552  11.00000  0.05    0.18
Q12   1   0.7576  0.2459  0.1138  11.00000  0.05    0.18
Q13   1   0.7857  0.3499  0.2523  11.00000  0.05    0.18
Q14   1   0.8065  0.2929  0.0398  11.00000  0.05    0.18
Q15   1   0.8981  0.4200  0.2801  11.00000  0.05    0.17
Q16   1   0.3988  0.0061  0.0285  11.00000  0.05    0.17
Q17   1   0.9127  0.2664  0.2810  11.00000  0.05    0.17
Q18   1   0.4475  0.2391  0.0059  11.00000  0.05    0.17
Q19   1   0.7899  0.2742  0.3274  11.00000  0.05    0.16
Q20   1   0.9102  0.4337  0.3268  11.00000  0.05    0.16
;
_shelx_res_checksum              5164

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c1_s         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.785 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c1_s         
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.64 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c1_s         
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.89 Ang.   
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c1_s         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 59 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT905_DMAFeF_c1_s         
;
PROBLEM: Negative K value in the Analysis of Variance ...     -0.277 Report
RESPONSE: The negative K value is only observed at the highest resolution
where the weakest reflections are observed.
;
_vrf_PLAT978_DMAFeF_c1_s         
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAMnF_c3_s
_database_code_depnum_ccdc_archive 'CCDC 1837764'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1791 0.2616 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.31888(17)
_cell_length_b                   8.31888(17)
_cell_length_c                   22.8731(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1370.84(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    220
_cell_measurement_theta_min      2.6290
_cell_measurement_theta_max      17.0320

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.323
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72711
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '0 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            775
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.092
_diffrn_reflns_theta_max         19.668
_diffrn_reflns_theta_full        14.283
_diffrn_measured_fraction_theta_max 0.492
_diffrn_measured_fraction_theta_full 0.822
_diffrn_reflns_Laue_measured_fraction_max 0.492
_diffrn_reflns_Laue_measured_fraction_full 0.822
_diffrn_reflns_point_group_measured_fraction_max 0.492
_diffrn_reflns_point_group_measured_fraction_full 0.822
_reflns_number_total             349
_reflns_number_gt                304
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+1.7090P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         349
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0687
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mn1 Mn 0.666667 0.333333 0.333333 0.0220(2) Uani 1 6 d S T P . .
N1 N 0.7540(10) 0.333333 0.083333 0.0424(17) Uani 0.3333 2 d DS T P . .
H3 H 0.757(8) 0.228(5) 0.080(4) 0.051 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0304(2) 0.0616(14) Uani 1 3 d DS T P . .
H2 H 0.548(3) 0.197(3) 0.0230(12) 0.074 Uiso 1 1 d D U . . .
O1 O 0.8772(2) 0.3230(2) 0.27908(6) 0.0377(4) Uani 1 1 d . . . . .
C1 C 1.000000 0.4519(3) 0.250000 0.0314(5) Uani 1 2 d S T P . .
H1 H 0.999999 0.563650 0.249999 0.038 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0221(3) 0.0221(3) 0.0219(3) 0.000 0.000 0.01103(13)
N1 0.035(3) 0.024(3) 0.064(4) -0.006(4) -0.003(2) 0.0119(15)
C2 0.069(2) 0.069(2) 0.047(2) 0.000 0.000 0.0345(11)
O1 0.0350(7) 0.0363(7) 0.0427(7) 0.0094(7) 0.0167(7) 0.0186(6)
C1 0.0279(12) 0.0286(8) 0.0375(11) 0.0004(6) 0.0009(12) 0.0140(6)

_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
Mn1 O1 2.1826(13) 31_655 ?
Mn1 O1 2.1826(13) 33_545 ?
Mn1 O1 2.1826(13) 3_665 ?
Mn1 O1 2.1826(13) 32 ?
Mn1 O1 2.1826(13) . ?
Mn1 O1 2.1826(13) 2_655 ?
N1 N1 1.258(14) 3_665 ?
N1 N1 1.258(14) 2_655 ?
N1 C2 1.411(6) 16_544 ?
N1 C2 1.411(6) . ?
O1 C1 1.2409(19) . ?

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 Mn1 O1 90.86(5) 31_655 33_545 ?
O1 Mn1 O1 89.14(5) 31_655 3_665 ?
O1 Mn1 O1 180.0 33_545 3_665 ?
O1 Mn1 O1 90.86(5) 31_655 32 ?
O1 Mn1 O1 90.86(5) 33_545 32 ?
O1 Mn1 O1 89.14(5) 3_665 32 ?
O1 Mn1 O1 180.00(5) 31_655 . ?
O1 Mn1 O1 89.14(5) 33_545 . ?
O1 Mn1 O1 90.86(5) 3_665 . ?
O1 Mn1 O1 89.14(5) 32 . ?
O1 Mn1 O1 89.14(5) 31_655 2_655 ?
O1 Mn1 O1 89.14(5) 33_545 2_655 ?
O1 Mn1 O1 90.86(5) 3_665 2_655 ?
O1 Mn1 O1 180.0 32 2_655 ?
O1 Mn1 O1 90.86(5) . 2_655 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 63.5(3) 3_665 16_544 ?
N1 N1 C2 63.5(3) 2_655 16_544 ?
N1 N1 C2 63.5(3) 3_665 . ?
N1 N1 C2 63.5(3) 2_655 . ?
C2 N1 C2 118.1(6) 16_544 . ?
N1 C2 N1 52.9(5) . 3_665 ?
N1 C2 N1 52.9(5) . 2_655 ?
N1 C2 N1 52.9(5) 3_665 2_655 ?
C1 O1 Mn1 126.96(15) . . ?
O1 C1 O1 126.3(3) . 6_765 ?

_refine_diff_density_max         0.231
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.057

_shelx_res_file                  
;
TITL DMAMnF_c3_s in R-3c
    DMAMnF_c3_s.res
    created by SHELXL-2016/6 at 18:21:40 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41119   8.318877   8.318877  22.873147  90.0000  90.0000 120.0000
ZERR    6.00   0.000174   0.000174   0.000278   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Mn
DISP $C -0.00006  0.00048  5.14212!source kissel
DISP $H -0.00003  0.00000  0.64130!source kissel
DISP $N  0.00062  0.00099  7.19266!source kissel
DISP $O  0.00180  0.00183 10.15895!source kissel
DISP $Mn  0.17908  0.26161 636.31605!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT -1 3 8
OMIT -1 1 4
TEMP 20
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.025600    1.709000
FVAR       3.13862
MOLE   1
MN1   5    0.666667    0.333333    0.333333    10.16667    0.02205    0.02205 =
         0.02191    0.00000    0.00000    0.01103
N1    3    0.753957    0.333333    0.083333    10.16667    0.03547    0.02379 =
         0.06404   -0.00623   -0.00311    0.01189
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.756819    0.227872    0.080400    10.33333   -1.20000
C2    1    0.666667    0.333333    0.030442    10.33333    0.06907    0.06907 =
         0.04675    0.00000    0.00000    0.03454
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.548192    0.197324    0.022959    11.00000   -1.20000
O1    4    0.877169    0.323045    0.279076    11.00000    0.03503    0.03632 =
         0.04273    0.00943    0.01670    0.01856
C1    1    1.000000    0.451856    0.250000    10.50000    0.02794    0.02863 =
         0.03747    0.00044    0.00089    0.01397
AFIX  43
H1    2    0.999999    0.563650    0.249999    10.50000   -1.20000
AFIX   0
HKLF 4




REM  DMAMnF_c3_s in R-3c
REM R1 =  0.0277 for     304 Fo > 4sig(Fo)  and  0.0329 for all     349 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0253      1.7661

REM Highest difference peak  0.231,  deepest hole -0.274,  1-sigma level  0.057
Q1    1   0.9252  0.4184  0.3074  11.00000  0.05    0.23
Q2    1   0.7981  0.3601  0.2930  11.00000  0.05    0.18
Q3    1   0.5323  0.2742  0.0341  11.00000  0.05    0.17
Q4    1   0.6200  0.2630 -0.0051  11.00000  0.05    0.17
Q5    1   0.7556  0.1275  0.1249  11.00000  0.05    0.17
Q6    1   0.6667  0.2473  0.0833  10.50000  0.05    0.14
Q7    1   0.9145  0.4853  0.3035  11.00000  0.05    0.14
Q8    1   0.8542  0.3491  0.2635  11.00000  0.05    0.14
Q9    1   0.7923  0.4688  0.3339  11.00000  0.05    0.14
Q10   1   0.9844  0.3870  0.2862  11.00000  0.05    0.13
Q11   1   1.0000  0.2977  0.2500  10.50000  0.05    0.13
Q12   1   0.6671  0.1335  0.0582  11.00000  0.05    0.13
Q13   1   0.4220  0.0005  0.0401  11.00000  0.05    0.11
Q14   1   0.9358  0.3075  0.0512  11.00000  0.05    0.11
Q15   1   1.0322  0.4579  0.3159  11.00000  0.05    0.11
Q16   1   0.7999  0.4195  0.2715  11.00000  0.05    0.11
Q17   1   0.4017  0.1782  0.0159  11.00000  0.05    0.10
Q18   1   1.0671  0.5938  0.2830  11.00000  0.05    0.10
Q19   1   0.8109  0.1758  0.2924  11.00000  0.05    0.10
Q20   1   0.9211  0.3627  0.3509  11.00000  0.05    0.10
;
_shelx_res_checksum              90122


# start Validation Reply Form
_vrf_PLAT029_DMAMnF_c3_s         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.822 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAMnF_c3_s         
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.85 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAMnF_c3_s         
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.58 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAMnF_c3_s         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 47 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT303_DMAMnF_c3_s         
;
PROBLEM: Full Occupancy Atom H2        with # Connections       1.33 Check 
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT978_DMAMnF_c3_s         
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMACuF_c4_p13
_database_code_depnum_ccdc_archive 'CCDC 1837748'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c4_p13       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.629 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT043_DMACuF_c4_p13       
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      11.08 Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT088_DMACuF_c4_p13       
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.92 Note
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired. In addition, there is a reduction in resolution for this pressure point, reducing the number of relections measured compared to the lower pressure points.
;
_vrf_PLAT911_DMACuF_c4_p13       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        253 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_CHEMW03_DMACuF_c4_p13       
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT041_DMACuF_c4_p13       
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT068_DMACuF_c4_p13       
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT148_DMACuF_c4_p13       
;
PROBLEM: s.u. on the      c    - Axis is (Too) Large ....      0.007 Ang.
RESPONSE: The diffraction spots are broader giving rise to larger errors in the unit cell parameters.
;
_vrf_PLAT155_DMACuF_c4_p13       
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The cell was kept in the given setting so as to be more comparable to the ambient phase unit cell.
;
_vrf_PLAT202_DMACuF_c4_p13       
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check
RESPONSE: Due to the many parameters in the refinement, refinement of isotropic thermal parameters were preffered.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4687 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.3066(17)
_cell_length_b                   5.849(2)
_cell_length_c                   5.599(7)
_cell_angle_alpha                96.76(8)
_cell_angle_beta                 88.11(6)
_cell_angle_gamma                95.53(3)
_cell_volume                     171.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    67
_cell_measurement_theta_min      4.4640
_cell_measurement_theta_max      12.7990

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_F_000             125
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.716
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.10110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '9.37 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            434
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.037
_diffrn_reflns_theta_max         14.921
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.614
_diffrn_measured_fraction_theta_full 0.629
_diffrn_reflns_Laue_measured_fraction_max 0.614
_diffrn_reflns_Laue_measured_fraction_full 0.629
_diffrn_reflns_point_group_measured_fraction_max 0.614
_diffrn_reflns_point_group_measured_fraction_full 0.629
_reflns_number_total             434
_reflns_number_gt                279
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1764P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         434
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0872
_refine_ls_wR_factor_ref         0.2522
_refine_ls_wR_factor_gt          0.2416
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0550(12) Uani 1 2 d S . P . .
O1 O 0.651(3) 0.634(4) 0.797(4) 0.059(5) Uiso 0.5 1 d . . P . .
O2 O 0.734(3) 0.570(4) 1.160(4) 0.063(5) Uiso 0.5 1 d . . P . .
O3 O -0.187(4) 0.608(5) 0.344(5) 0.068(6) Uiso 0.5 1 d . . P . .
O4 O 0.222(4) 0.596(5) 0.356(5) 0.072(6) Uiso 0.5 1 d . . P . .
O5 O 0.315(4) -0.174(5) 0.417(5) 0.078(6) Uiso 0.5 1 d . . P . .
O6 O 0.358(4) 0.199(5) 0.389(5) 0.066(5) Uiso 0.5 1 d . . P . .
C1 C 0.595(4) 0.537(6) 0.986(5) 0.049(6) Uiso 0.5 1 d . . P . .
C3 C 0.431(4) 0.015(5) 0.465(6) 0.051(7) Uiso 0.5 1 d . . P . .
C2 C 0.010(4) 0.549(4) 0.431(4) 0.039(6) Uiso 0.5 1 d . . P . .
C4 C 0.178(4) -0.090(5) 0.943(5) 0.105(7) Uiso 1 1 d . . . . .
N1 N 0.000(4) -0.027(5) 1.086(4) 0.058(6) Uiso 0.5 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0565(15) 0.058(2) 0.0439(18) -0.0117(18) -0.0113(9) -0.0121(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
Cu1 O4 1.87(2) 2_666 ?
Cu1 O4 1.87(2) . ?
Cu1 O6 1.89(3) 2_666 ?
Cu1 O6 1.89(3) . ?
Cu1 O1 1.92(2) 2_666 ?
Cu1 O1 1.92(2) . ?
Cu1 O3 1.94(2) 2_566 ?
Cu1 O3 1.94(2) 1_655 ?
Cu1 O2 2.29(2) 1_554 ?
Cu1 O2 2.29(2) 2_667 ?
Cu1 O5 2.33(3) 1_565 ?
Cu1 O5 2.33(3) 2_656 ?
O1 C1 1.27(3) . ?
O1 O6 1.51(3) 2_666 ?
O1 O4 1.69(4) 2_666 ?
O2 O3 1.11(3) 1_656 ?
O2 C1 1.23(3) . ?
O3 C2 1.26(3) . ?
O4 C2 1.21(3) . ?
O4 O5 1.40(4) 1_565 ?
O4 C2 1.90(3) 2_566 ?
O5 C3 1.22(4) . ?
O5 C3 1.67(4) 2_656 ?
O6 C3 1.30(4) . ?
C1 C1 1.07(5) 2_667 ?
C3 C3 0.88(4) 2_656 ?
C2 C2 1.01(4) 2_566 ?
C4 N1 1.24(3) 2_557 ?
C4 N1 1.27(4) . ?
N1 N1 1.05(4) 2_557 ?

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
O4 Cu1 O4 180.0 2_666 . ?
O4 Cu1 O6 84.3(11) 2_666 2_666 ?
O4 Cu1 O6 95.7(11) . 2_666 ?
O4 Cu1 O6 95.7(11) 2_666 . ?
O4 Cu1 O6 84.3(11) . . ?
O6 Cu1 O6 180.0(12) 2_666 . ?
O4 Cu1 O1 127.0(11) 2_666 2_666 ?
O4 Cu1 O1 53.0(11) . 2_666 ?
O6 Cu1 O1 133.3(10) 2_666 2_666 ?
O6 Cu1 O1 46.7(10) . 2_666 ?
O4 Cu1 O1 53.0(11) 2_666 . ?
O4 Cu1 O1 127.0(11) . . ?
O6 Cu1 O1 46.7(10) 2_666 . ?
O6 Cu1 O1 133.3(10) . . ?
O1 Cu1 O1 180.0 2_666 . ?
O4 Cu1 O3 110.7(9) 2_666 2_566 ?
O4 Cu1 O3 69.3(9) . 2_566 ?
O6 Cu1 O3 116.6(11) 2_666 2_566 ?
O6 Cu1 O3 63.4(11) . 2_566 ?
O1 Cu1 O3 86.5(10) 2_666 2_566 ?
O1 Cu1 O3 93.5(9) . 2_566 ?
O4 Cu1 O3 69.3(9) 2_666 1_655 ?
O4 Cu1 O3 110.7(9) . 1_655 ?
O6 Cu1 O3 63.4(11) 2_666 1_655 ?
O6 Cu1 O3 116.6(11) . 1_655 ?
O1 Cu1 O3 93.5(9) 2_666 1_655 ?
O1 Cu1 O3 86.5(10) . 1_655 ?
O3 Cu1 O3 180.0 2_566 1_655 ?
O4 Cu1 O2 92.0(9) 2_666 1_554 ?
O4 Cu1 O2 88.0(9) . 1_554 ?
O6 Cu1 O2 82.4(10) 2_666 1_554 ?
O6 Cu1 O2 97.6(10) . 1_554 ?
O1 Cu1 O2 65.0(8) 2_666 1_554 ?
O1 Cu1 O2 115.0(8) . 1_554 ?
O3 Cu1 O2 151.0(8) 2_566 1_554 ?
O3 Cu1 O2 29.0(8) 1_655 1_554 ?
O4 Cu1 O2 88.0(9) 2_666 2_667 ?
O4 Cu1 O2 92.0(9) . 2_667 ?
O6 Cu1 O2 97.6(10) 2_666 2_667 ?
O6 Cu1 O2 82.4(10) . 2_667 ?
O1 Cu1 O2 115.0(8) 2_666 2_667 ?
O1 Cu1 O2 65.0(8) . 2_667 ?
O3 Cu1 O2 29.0(8) 2_566 2_667 ?
O3 Cu1 O2 151.0(8) 1_655 2_667 ?
O2 Cu1 O2 180.0 1_554 2_667 ?
O4 Cu1 O5 143.1(11) 2_666 1_565 ?
O4 Cu1 O5 36.9(11) . 1_565 ?
O6 Cu1 O5 58.8(9) 2_666 1_565 ?
O6 Cu1 O5 121.2(9) . 1_565 ?
O1 Cu1 O5 83.1(10) 2_666 1_565 ?
O1 Cu1 O5 96.9(10) . 1_565 ?
O3 Cu1 O5 89.6(10) 2_566 1_565 ?
O3 Cu1 O5 90.4(10) 1_655 1_565 ?
O2 Cu1 O5 81.9(8) 1_554 1_565 ?
O2 Cu1 O5 98.1(8) 2_667 1_565 ?
O4 Cu1 O5 36.9(11) 2_666 2_656 ?
O4 Cu1 O5 143.1(11) . 2_656 ?
O6 Cu1 O5 121.2(9) 2_666 2_656 ?
O6 Cu1 O5 58.8(9) . 2_656 ?
O1 Cu1 O5 96.9(10) 2_666 2_656 ?
O1 Cu1 O5 83.1(10) . 2_656 ?
O3 Cu1 O5 90.4(10) 2_566 2_656 ?
O3 Cu1 O5 89.6(10) 1_655 2_656 ?
O2 Cu1 O5 98.1(8) 1_554 2_656 ?
O2 Cu1 O5 81.9(8) 2_667 2_656 ?
O5 Cu1 O5 180.0 1_565 2_656 ?
C1 O1 O6 159(2) . 2_666 ?
C1 O1 O4 95(2) . 2_666 ?
O6 O1 O4 103.9(17) 2_666 2_666 ?
C1 O1 Cu1 118.7(18) . . ?
O6 O1 Cu1 65.7(12) 2_666 . ?
O4 O1 Cu1 62.0(12) 2_666 . ?
O3 O2 C1 165(3) 1_656 . ?
O3 O2 Cu1 57.5(14) 1_656 1_556 ?
C1 O2 Cu1 109.1(16) . 1_556 ?
O2 O3 C2 131(3) 1_454 . ?
O2 O3 Cu1 93.5(16) 1_454 1_455 ?
C2 O3 Cu1 114.3(18) . 1_455 ?
C2 O4 O5 114(3) . 1_565 ?
C2 O4 O1 113(2) . 2_666 ?
O5 O4 O1 133.0(19) 1_565 2_666 ?
C2 O4 Cu1 120(2) . . ?
O5 O4 Cu1 89.8(15) 1_565 . ?
O1 O4 Cu1 65.0(11) 2_666 . ?
C2 O4 C2 28.3(16) . 2_566 ?
O5 O4 C2 119(2) 1_565 2_566 ?
O1 O4 C2 101.7(16) 2_666 2_566 ?
Cu1 O4 C2 92.2(13) . 2_566 ?
C3 O5 O4 171(3) . 1_545 ?
C3 O5 C3 31(2) . 2_656 ?
O4 O5 C3 141(2) 1_545 2_656 ?
C3 O5 Cu1 118.6(17) . 1_545 ?
O4 O5 Cu1 53.4(13) 1_545 1_545 ?
C3 O5 Cu1 87.8(14) 2_656 1_545 ?
C3 O6 O1 153(3) . 2_666 ?
C3 O6 Cu1 122.3(18) . . ?
O1 O6 Cu1 67.6(13) 2_666 . ?
C1 C1 O2 117(4) 2_667 . ?
C1 C1 O1 120(4) 2_667 . ?
O2 C1 O1 121(2) . . ?
C3 C3 O5 104(5) 2_656 . ?
C3 C3 O6 134(5) 2_656 . ?
O5 C3 O6 121(2) . . ?
C3 C3 O5 45(3) 2_656 2_656 ?
O5 C3 O5 149(2) . 2_656 ?
O6 C3 O5 89(2) . 2_656 ?
C2 C2 O4 117(3) 2_566 . ?
C2 C2 O3 119(3) 2_566 . ?
O4 C2 O3 124(2) . . ?
C2 C2 O4 34.6(19) 2_566 2_566 ?
O4 C2 O4 151.7(16) . 2_566 ?
O3 C2 O4 84.1(15) . 2_566 ?
N1 C4 N1 49(2) 2_557 . ?
N1 N1 C4 67(3) 2_557 2_557 ?
N1 N1 C4 64(3) 2_557 . ?
C4 N1 C4 131(2) 2_557 . ?

_refine_diff_density_max         0.810
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.143

_shelx_res_file                  
;
TITL DMACuF_c4_p13_s_twin in P-1
    DMACuF_c4_p13_reslim0p8_mask1p5_rfxy_twin1_hklf5.res
    created by SHELXL-2016/6 at 16:52:29 on 21-Mar-2018
REM P-1 (#2 in standard setting)
CELL 0.41108    5.306615 5.849475  5.599299     96.7646  88.1056  95.5295
ZERR    1.00    0.001694 0.002179   0.007074     0.0823  0.0606    0.0302
LATT  1
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.14091!source kissel
DISP $H -0.00003  0.00000  0.64127!source kissel
DISP $N  0.00062  0.00099  7.19030!source kissel
DISP $O  0.00180  0.00183 10.15475!source kissel
DISP $Cu  0.24634  0.46870 1129.00277!source kissel
UNIT 5.00 11.00 1.00 6.00 1.00
OMIT 4 5 1
OMIT -4 -5 -1
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
SIZE 0.03 0.03 0.015
ACTA
BOND
FMAP 2
PLAN 20
MERG 0
WGHT    0.176400
BASF   0.55569
FVAR       5.13668
MOLE   1
CU1   5    0.500000    0.500000    0.500000    10.50000    0.05647    0.05780 =
         0.04388   -0.01170   -0.01128   -0.01213
O1    4    0.650805    0.633950    0.796706    10.50000    0.05869
O2    4    0.734426    0.569982    1.160123    10.50000    0.06290
O3    4   -0.186547    0.607740    0.343951    10.50000    0.06819
O4    4    0.222165    0.595792    0.355728    10.50000    0.07195
O5    4    0.315376   -0.174064    0.416737    10.50000    0.07839
O6    4    0.357657    0.199409    0.388667    10.50000    0.06645
C1    1    0.595022    0.537352    0.985738    10.50000    0.04933
C3    1    0.431157    0.015030    0.464948    10.50000    0.05095
C2    1    0.009713    0.549069    0.431320    10.50000    0.03872
C4    1    0.177801   -0.090395    0.943490    11.00000    0.10543
N1    3   -0.000271   -0.026526    1.086164    10.50000    0.05770
MOLE   2
HKLF 5 1 0 1 0 1 0 0 0 0 1 1 0




REM  DMACuF_c4_p13_s_twin in P-1
REM R1 =  0.0872 for     279 Fo > 4sig(Fo)  and  0.1088 for all     434 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.1764      0.0000

REM Highest difference peak  0.810,  deepest hole -0.508,  1-sigma level  0.143
Q1    1   0.3343  0.5393  0.4973  11.00000  0.05    0.81
Q2    1   0.4989  0.4777  0.6692  11.00000  0.05    0.52
Q3    1   0.1367 -0.0127  0.8558  11.00000  0.05    0.51
Q4    1   0.4993  0.6732  0.5079  11.00000  0.05    0.47
Q5    1   0.6945  0.6277  0.9851  11.00000  0.05    0.44
Q6    1   0.4200  0.1665  0.5417  11.00000  0.05    0.43
Q7    1   0.1057 -0.1189  1.2380  11.00000  0.05    0.41
Q8    1   0.3371  0.0099  0.4249  11.00000  0.05    0.39
Q9    1   0.3842  0.1661  0.5918  11.00000  0.05    0.37
Q10   1   0.5847  0.3786  0.9793  11.00000  0.05    0.36
Q11   1   0.2351  0.0364  0.5331  11.00000  0.05    0.36
Q12   1   0.3681 -0.1276  0.9844  11.00000  0.05    0.34
Q13   1   0.6177  0.3270  1.0012  11.00000  0.05    0.33
Q14   1   0.2908  0.4991  0.2981  11.00000  0.05    0.33
Q15   1  -0.0037  0.0280  1.0400  11.00000  0.05    0.32
Q16   1   0.0654 -0.0147  0.4798  11.00000  0.05    0.31
Q17   1   0.4618  0.0022  0.5268  11.00000  0.05    0.31
Q18   1  -0.1332  0.5326  0.2629  11.00000  0.05    0.30
Q19   1   0.7513  0.4198  1.1933  11.00000  0.05    0.30
Q20   1   0.6215  0.6512  1.1640  11.00000  0.05    0.29
;
_shelx_res_checksum              1611
####################################################################### 
# 
# 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_DMAFeF_c2_p03
_database_code_depnum_ccdc_archive 'CCDC 1837757'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.0626(4)
_cell_length_b                   8.0626(4)
_cell_length_c                   21.3349(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1201.07(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    225
_cell_measurement_theta_min      2.9240
_cell_measurement_theta_max      16.3390

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.420
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '3.13 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            764
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.923
_diffrn_reflns_theta_max         19.192
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.469
_diffrn_measured_fraction_theta_full 0.721
_diffrn_reflns_Laue_measured_fraction_max 0.469
_diffrn_reflns_Laue_measured_fraction_full 0.721
_diffrn_reflns_point_group_measured_fraction_max 0.469
_diffrn_reflns_point_group_measured_fraction_full 0.721
_reflns_number_total             271
_reflns_number_gt                224
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0436P)²+4.4349P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         271
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0309(4) Uani 1 6 d S T P . .
N1 N 0.7454(19) 0.333333 0.083333 0.052(4) Uani 0.3333 2 d DS T P . .
H3 H 0.776(9) 0.241(7) 0.087(9) 0.063 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0267(5) 0.065(2) Uani 1 3 d DS T P . .
H2 H 0.541(5) 0.247(6) -0.003(2) 0.078 Uiso 1 1 d D U . . .
O1 O 0.8683(4) 0.3089(4) 0.27809(13) 0.0443(7) Uani 1 1 d . . . . .
C1 C 1.000000 0.4458(6) 0.250000 0.0372(10) Uani 1 2 d S T P . .
H1 H 1.000000 0.561193 0.249999 0.045 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0309(5) 0.0309(5) 0.0310(7) 0.000 0.000 0.0155(3)
N1 0.043(6) 0.036(7) 0.075(12) -0.007(8) -0.003(4) 0.018(4)
C2 0.080(4) 0.080(4) 0.036(5) 0.000 0.000 0.040(2)
O1 0.0439(15) 0.0416(15) 0.0483(16) 0.0048(11) 0.0133(11) 0.0221(12)
C1 0.036(3) 0.0346(18) 0.041(3) 0.0003(9) 0.0006(18) 0.0181(13)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.096(2) . ?
Fe1 O1 2.096(2) 31_655 ?
Fe1 O1 2.096(2) 33_545 ?
Fe1 O1 2.096(2) 3_665 ?
Fe1 O1 2.096(2) 32 ?
Fe1 O1 2.096(2) 2_655 ?
N1 N1 1.10(3) 3_665 ?
N1 N1 1.10(3) 2_655 ?
N1 C2 1.364(11) 16_544 ?
N1 C2 1.365(11) . ?
O1 C1 1.238(3) . ?

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 Fe1 O1 180.00(15) . 31_655 ?
O1 Fe1 O1 88.54(11) . 33_545 ?
O1 Fe1 O1 91.46(11) 31_655 33_545 ?
O1 Fe1 O1 91.46(11) . 3_665 ?
O1 Fe1 O1 88.54(11) 31_655 3_665 ?
O1 Fe1 O1 180.0 33_545 3_665 ?
O1 Fe1 O1 88.54(11) . 32 ?
O1 Fe1 O1 91.46(11) 31_655 32 ?
O1 Fe1 O1 91.46(11) 33_545 32 ?
O1 Fe1 O1 88.54(11) 3_665 32 ?
O1 Fe1 O1 91.46(11) . 2_655 ?
O1 Fe1 O1 88.54(11) 31_655 2_655 ?
O1 Fe1 O1 88.54(11) 33_545 2_655 ?
O1 Fe1 O1 91.46(11) 3_665 2_655 ?
O1 Fe1 O1 180.0 32 2_655 ?
N1 N1 N1 60.000(1) 3_665 2_655 ?
N1 N1 C2 66.2(5) 3_665 16_544 ?
N1 N1 C2 66.2(5) 2_655 16_544 ?
N1 N1 C2 66.2(5) 3_665 . ?
N1 N1 C2 66.2(5) 2_655 . ?
C2 N1 C2 124.6(12) 16_544 . ?
N1 C2 N1 47.5(10) . 3_665 ?
N1 C2 N1 47.5(10) . 2_655 ?
N1 C2 N1 47.5(10) 3_665 2_655 ?
C1 O1 Fe1 123.2(2) . . ?
O1 C1 O1 124.8(4) 6_765 . ?

_refine_diff_density_max         0.336
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.070

_shelx_res_file                  
;
TITL DMAFeF_c2_p03_s_ModelR in R-3c
    DMAFeF_c2_p03_s_ModelR.res
    created by SHELXL-2016/6 at 15:16:32 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41111   8.062559   8.062559  21.334911  90.0000  90.0000 120.0000
ZERR    6.00   0.000397   0.000397   0.001114   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 0 2 4
OMIT 0 1 2
ACTA

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.043600    4.434900
FVAR       3.40701
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.03091    0.03091 =
         0.03097    0.00000    0.00000    0.01545
N1    3    0.745391    0.333333    0.083333    10.16667    0.04338    0.03621 =
         0.07507   -0.00653   -0.00327    0.01811
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.776183    0.240950    0.086706    10.33333   -1.20000
C2    1    0.666667    0.333333    0.026715    10.33333    0.07979    0.07979 =
         0.03605    0.00000    0.00000    0.03989
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.540651    0.247496   -0.002506    11.00000   -1.20000
O1    4    0.868329    0.308884    0.278086    11.00000    0.04389    0.04156 =
         0.04834    0.00483    0.01327    0.02209
C1    1    1.000000    0.445846    0.250000    10.50000    0.03628    0.03461 =
         0.04117    0.00032    0.00064    0.01814
AFIX  43
H1    2    1.000000    0.561193    0.249999    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c2_p03_s_ModelR in R-3c
REM R1 =  0.0433 for     224 Fo > 4sig(Fo)  and  0.0543 for all     271 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0435      4.3187

REM Highest difference peak  0.336,  deepest hole -0.337,  1-sigma level  0.070
Q1    1   0.7264  0.2604  0.3519  11.00000  0.05    0.32
Q2    1   0.8793  0.5724  0.2808  11.00000  0.05    0.29
Q3    1   0.7531  0.2529  0.3037  11.00000  0.05    0.25
Q4    1   1.1840  0.6887  0.2512  11.00000  0.05    0.22
Q5    1   0.9190  0.3670  0.3070  11.00000  0.05    0.22
Q6    1   0.8296  0.2811  0.1364  11.00000  0.05    0.22
Q7    1   0.8067  0.3014  0.3128  11.00000  0.05    0.21
Q8    1   0.7134  0.2722  0.2828  11.00000  0.05    0.19
Q9    1   0.5872  0.3489 -0.0236  11.00000  0.05    0.19
Q10   1   0.7855  0.3284  0.2662  11.00000  0.05    0.18
Q11   1   0.8875  0.4546  0.2930  11.00000  0.05    0.18
Q12   1   0.4799  0.4143 -0.0191  11.00000  0.05    0.17
Q13   1   0.7017  0.1399  0.0606  11.00000  0.05    0.17
Q14   1   0.6011  0.3124 -0.0751  11.00000  0.05    0.17
Q15   1   0.6000  0.2096  0.0174  11.00000  0.05    0.16
Q16   1   0.9542  0.3498  0.3461  11.00000  0.05    0.16
Q17   1   0.6667  0.3333 -0.0140  10.33333  0.05    0.16
Q18   1   0.5743  0.1604 -0.0373  11.00000  0.05    0.15
Q19   1   0.8921  0.2148  0.2895  11.00000  0.05    0.15
Q20   1   1.0454  0.6051  0.2825  11.00000  0.05    0.15
;
_shelx_res_checksum              1744

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c2_p03       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.721 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c2_p03       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.56 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c2_p03       
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               2.00 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c2_p03       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 66 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT088_DMAFeF_c2_p03       
;
PROBLEM: Poor Data / Parameter Ratio ....................       8.74 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. Additionally,
the positioning of the hydrogen atoms for the dynamically disordered 
(CH3)2NH2 unit could not be performed with standard AFIX commands. Instead
distance restraints are used which increases the number of parameters as the
hydrogen positions are refined.
;
_vrf_PLAT978_DMAFeF_c2_p03       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAFeF_c2_p02
_database_code_depnum_ccdc_archive 'CCDC 1837756'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.1069(2)
_cell_length_b                   8.1069(2)
_cell_length_c                   21.6257(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1230.87(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    314
_cell_measurement_theta_min      2.9070
_cell_measurement_theta_max      17.2920

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.410
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '2.12 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            780
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.335
_diffrn_reflns_theta_max         19.724
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.441
_diffrn_measured_fraction_theta_full 0.722
_diffrn_reflns_Laue_measured_fraction_max 0.441
_diffrn_reflns_Laue_measured_fraction_full 0.722
_diffrn_reflns_point_group_measured_fraction_max 0.441
_diffrn_reflns_point_group_measured_fraction_full 0.722
_reflns_number_total             282
_reflns_number_gt                250
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0267P)²+3.6268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         282
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0793
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_restrained_S_all      1.205
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0255(3) Uani 1 6 d S T P . .
N1 N 0.7483(15) 0.333333 0.083333 0.049(3) Uani 0.3333 2 d DS T P . .
H3 H 0.781(9) 0.248(9) 0.096(6) 0.059 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0274(3) 0.0601(18) Uani 1 3 d DS T P . .
H2 H 0.536(4) 0.241(5) 0.0024(19) 0.072 Uiso 1 1 d D U . . .
O1 O 0.8703(3) 0.3135(3) 0.27823(10) 0.0392(5) Uani 1 1 d . . . . .
C1 C 1.000000 0.4485(5) 0.250000 0.0340(8) Uani 1 2 d S T P . .
H1 H 1.000002 0.563228 0.250000 0.041 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0242(4) 0.0242(4) 0.0280(5) 0.000 0.000 0.01211(19)
N1 0.039(4) 0.029(6) 0.076(9) -0.006(6) -0.003(3) 0.014(3)
C2 0.071(3) 0.071(3) 0.039(4) 0.000 0.000 0.0353(15)
O1 0.0368(12) 0.0345(11) 0.0454(12) 0.0040(8) 0.0124(8) 0.0171(9)
C1 0.029(2) 0.0309(15) 0.041(2) 0.0011(7) 0.0022(15) 0.0147(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
Fe1 O1 2.1061(19) 31_655 ?
Fe1 O1 2.1062(19) . ?
Fe1 O1 2.1061(19) 33_545 ?
Fe1 O1 2.1062(19) 3_665 ?
Fe1 O1 2.1062(19) 32 ?
Fe1 O1 2.1062(19) 2_655 ?
N1 N1 1.15(2) 3_665 ?
N1 N1 1.15(2) 2_655 ?
N1 C2 1.379(9) 16_544 ?
N1 C2 1.379(9) . ?
O1 C1 1.235(3) . ?

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 Fe1 O1 180.0 31_655 . ?
O1 Fe1 O1 91.14(9) 31_655 33_545 ?
O1 Fe1 O1 88.86(9) . 33_545 ?
O1 Fe1 O1 88.86(9) 31_655 3_665 ?
O1 Fe1 O1 91.14(9) . 3_665 ?
O1 Fe1 O1 180.0 33_545 3_665 ?
O1 Fe1 O1 91.14(9) 31_655 32 ?
O1 Fe1 O1 88.86(9) . 32 ?
O1 Fe1 O1 91.14(9) 33_545 32 ?
O1 Fe1 O1 88.86(9) 3_665 32 ?
O1 Fe1 O1 88.86(9) 31_655 2_655 ?
O1 Fe1 O1 91.14(9) . 2_655 ?
O1 Fe1 O1 88.86(9) 33_545 2_655 ?
O1 Fe1 O1 91.14(9) 3_665 2_655 ?
O1 Fe1 O1 180.0 32 2_655 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 65.4(4) 3_665 16_544 ?
N1 N1 C2 65.4(4) 2_655 16_544 ?
N1 N1 C2 65.4(4) 3_665 . ?
N1 N1 C2 65.4(4) 2_655 . ?
C2 N1 C2 122.6(9) 16_544 . ?
N1 C2 N1 49.1(8) . 3_665 ?
N1 C2 N1 49.1(8) . 2_655 ?
N1 C2 N1 49.1(8) 3_665 2_655 ?
C1 O1 Fe1 124.4(2) . . ?
O1 C1 O1 125.2(4) 6_765 . ?

_refine_diff_density_max         0.282
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.065

_shelx_res_file                  
;
TITL DMAFeF_c2_p02_s_ModelR in R-3c
    DMAFeF_c2_p02_s_ModelR.res
    created by SHELXL-2016/6 at 15:02:48 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41111   8.106916   8.106916  21.625687  90.0000  90.0000 120.0000
ZERR    6.00   0.000214   0.000214   0.000776   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT -1 2 0
OMIT 0 2 4
OMIT 0 1 2
ACTA

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.026700    3.626800
FVAR       3.36689
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.02422    0.02422 =
         0.02801    0.00000    0.00000    0.01211
N1    3    0.748340    0.333333    0.083333    10.16667    0.03879    0.02853 =
         0.07574   -0.00562   -0.00281    0.01426
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.781324    0.247989    0.095684    10.33333   -1.20000
C2    1    0.666667    0.333333    0.027406    10.33333    0.07063    0.07063 =
         0.03890    0.00000    0.00000    0.03532
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.536180    0.241427    0.002376    11.00000   -1.20000
O1    4    0.870268    0.313481    0.278232    11.00000    0.03678    0.03452 =
         0.04536    0.00404    0.01237    0.01715
C1    1    1.000000    0.448510    0.250000    10.50000    0.02935    0.03089 =
         0.04125    0.00108    0.00216    0.01468
AFIX  43
H1    2    1.000002    0.563228    0.250000    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c2_p02_s_ModelR in R-3c
REM R1 =  0.0351 for     250 Fo > 4sig(Fo)  and  0.0407 for all     282 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0267      3.6290

REM Highest difference peak  0.282,  deepest hole -0.297,  1-sigma level  0.065
Q1    1   1.0686  0.5921  0.2834  11.00000  0.05    0.28
Q2    1   0.8961  0.3643  0.3099  11.00000  0.05    0.22
Q3    1   0.7654  0.4723  0.3512  11.00000  0.05    0.22
Q4    1   0.6667  0.3333  0.0579  10.33333  0.05    0.19
Q5    1   0.9432  0.4049  0.2760  11.00000  0.05    0.19
Q6    1   0.7377  0.2428  0.3018  11.00000  0.05    0.19
Q7    1   0.4834  0.1957  0.0392  11.00000  0.05    0.18
Q8    1   0.8040  0.3242  0.2622  11.00000  0.05    0.18
Q9    1   0.6667  0.3333 -0.0090  10.33333  0.05    0.17
Q10   1   0.7142  0.1550  0.0697  11.00000  0.05    0.17
Q11   1   0.8790  0.4430  0.2925  11.00000  0.05    0.17
Q12   1   0.9790  0.2797  0.2833  11.00000  0.05    0.17
Q13   1   1.0046  0.3464  0.3205  11.00000  0.05    0.16
Q14   1   0.6013  0.2185  0.0151  11.00000  0.05    0.16
Q15   1   0.4844  0.1190  0.0262  11.00000  0.05    0.16
Q16   1   0.8908  0.5711  0.2813  11.00000  0.05    0.15
Q17   1   1.1012  0.7188  0.2626  11.00000  0.05    0.14
Q18   1   0.9038  0.2477  0.3316  11.00000  0.05    0.14
Q19   1   0.5564  0.3416 -0.0213  11.00000  0.05    0.14
Q20   1   0.6774  0.2004  0.2631  11.00000  0.05    0.14
;
_shelx_res_checksum              48708

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c2_p02       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.722 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c2_p02       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.63 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c2_p02       
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.75 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c2_p02       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 66 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT088_DMAFeF_c2_p02       
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.10 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. Additionally,
the positioning of the hydrogen atoms for the dynamically disordered 
(CH3)2NH2 unit could not be performed with standard AFIX commands. Instead
distance restraints are used which increases the number of parameters as the
hydrogen positions are refined.
;
_vrf_PLAT913_DMAFeF_c2_p02       
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....          4 Note  
RESPONSE: The overflow reflections were omitted from the refinement.
;
_vrf_PLAT978_DMAFeF_c2_p02       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAFeF_c2_p05
_database_code_depnum_ccdc_archive 'CCDC 1837759'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   7.9888(10)
_cell_length_b                   7.9888(10)
_cell_length_c                   20.926(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1156.6(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    142
_cell_measurement_theta_min      2.9510
_cell_measurement_theta_max      14.5860

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.436
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80762
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '4.68 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            741
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.950
_diffrn_reflns_theta_max         19.478
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.458
_diffrn_measured_fraction_theta_full 0.725
_diffrn_reflns_Laue_measured_fraction_max 0.458
_diffrn_reflns_Laue_measured_fraction_full 0.725
_diffrn_reflns_point_group_measured_fraction_max 0.458
_diffrn_reflns_point_group_measured_fraction_full 0.725
_reflns_number_total             267
_reflns_number_gt                191
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0656P)²+5.4456P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         267
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1556
_refine_ls_wR_factor_gt          0.1345
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0445(6) Uani 1 6 d S T P . .
N1 N 0.742(3) 0.333333 0.083333 0.080(8) Uani 0.3333 2 d DS T P . .
H3 H 0.793(15) 0.27(3) 0.105(8) 0.096 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0257(6) 0.080(4) Uani 1 3 d DS T P . .
H2 H 0.540(6) 0.252(8) -0.005(3) 0.096 Uiso 1 1 d D U . . .
O1 O 0.8658(5) 0.3040(5) 0.27754(17) 0.0580(10) Uani 1 1 d . . . . .
C1 C 1.000000 0.4423(10) 0.250000 0.0513(15) Uani 1 2 d S T P . .
H1 H 1.000001 0.558716 0.250002 0.062 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0476(8) 0.0476(8) 0.0381(10) 0.000 0.000 0.0238(4)
N1 0.064(10) 0.064(12) 0.11(3) -0.010(16) -0.005(8) 0.032(6)
C2 0.102(7) 0.102(7) 0.035(6) 0.000 0.000 0.051(3)
O1 0.061(2) 0.058(2) 0.056(2) 0.0043(15) 0.0132(16) 0.0306(17)
C1 0.052(4) 0.058(3) 0.042(4) 0.0019(13) 0.004(3) 0.0259(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
Fe1 O1 2.078(3) 31_655 ?
Fe1 O1 2.078(3) 33_545 ?
Fe1 O1 2.078(3) 3_665 ?
Fe1 O1 2.078(3) 32 ?
Fe1 O1 2.078(3) 2_655 ?
Fe1 O1 2.078(3) . ?
N1 N1 1.05(4) 3_665 ?
N1 N1 1.05(4) 2_655 ?
N1 C2 1.348(14) 16_544 ?
N1 C2 1.348(14) . ?
O1 C1 1.232(5) . ?

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 Fe1 O1 91.53(15) 31_655 33_545 ?
O1 Fe1 O1 88.47(15) 31_655 3_665 ?
O1 Fe1 O1 180.0 33_545 3_665 ?
O1 Fe1 O1 91.53(15) 31_655 32 ?
O1 Fe1 O1 91.53(15) 33_545 32 ?
O1 Fe1 O1 88.47(15) 3_665 32 ?
O1 Fe1 O1 88.47(15) 31_655 2_655 ?
O1 Fe1 O1 88.47(15) 33_545 2_655 ?
O1 Fe1 O1 91.53(15) 3_665 2_655 ?
O1 Fe1 O1 180.0 32 2_655 ?
O1 Fe1 O1 180.0 31_655 . ?
O1 Fe1 O1 88.47(15) 33_545 . ?
O1 Fe1 O1 91.53(15) 3_665 . ?
O1 Fe1 O1 88.47(15) 32 . ?
O1 Fe1 O1 91.53(15) 2_655 . ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 67.2(7) 3_665 16_544 ?
N1 N1 C2 67.2(7) 2_655 16_544 ?
N1 N1 C2 67.2(7) 3_665 . ?
N1 N1 C2 67.2(7) 2_655 . ?
C2 N1 C2 126.8(18) 16_544 . ?
N1 C2 N1 45.6(15) . 3_665 ?
N1 C2 N1 45.6(15) . 2_655 ?
N1 C2 N1 45.6(15) 3_665 2_655 ?
C1 O1 Fe1 122.3(4) . . ?
O1 C1 O1 125.1(7) . 6_765 ?

_refine_diff_density_max         0.470
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.080

_shelx_res_file                  
;
TITL DMAFeF_c2_p05_s_ModelR in R-3c
    DMAFeF_c2_p05_s_ModelR.res
    created by SHELXL-2016/6 at 15:31:25 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41111   7.988759   7.988759  20.926262  90.0000  90.0000 120.0000
ZERR    6.00   0.000984   0.000984   0.002301   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 0 2 4
OMIT 0 1 2
ACTA

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.065600    5.445600
FVAR       3.54578
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.04764    0.04764 =
         0.03807    0.00000    0.00000    0.02382
N1    3    0.742237    0.333333    0.083333    10.16667    0.06358    0.06394 =
         0.11265   -0.00963   -0.00481    0.03197
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.793313    0.272373    0.105074    10.33333   -1.20000
C2    1    0.666667    0.333333    0.025730    10.33333    0.10215    0.10215 =
         0.03500    0.00000    0.00000    0.05107
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.539736    0.251823   -0.004985    11.00000   -1.20000
O1    4    0.865756    0.304047    0.277539    11.00000    0.06082    0.05813 =
         0.05602    0.00432    0.01322    0.03058
C1    1    1.000000    0.442302    0.250000    10.50000    0.05179    0.05760 =
         0.04246    0.00187    0.00375    0.02590
AFIX  43
H1    2    1.000001    0.558716    0.250002    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c2_p05_s_ModelR in R-3c
REM R1 =  0.0549 for     191 Fo > 4sig(Fo)  and  0.0737 for all     267 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0656      5.4411

REM Highest difference peak  0.470,  deepest hole -0.443,  1-sigma level  0.080
Q1    1   0.8731  0.5765  0.2769  11.00000  0.05    0.37
Q2    1   0.7636  0.2499  0.3078  11.00000  0.05    0.36
Q3    1   0.8404  0.4184  0.3107  11.00000  0.05    0.32
Q4    1   0.8306  0.4943  0.2531  11.00000  0.05    0.25
Q5    1   0.9238  0.4723  0.2944  11.00000  0.05    0.24
Q6    1   0.6667  0.1249  0.0833  10.50000  0.05    0.23
Q7    1   0.7797  0.2487  0.1368  11.00000  0.05    0.21
Q8    1   0.7607  0.3393  0.2790  11.00000  0.05    0.20
Q9    1   0.6144  0.3517 -0.0295  11.00000  0.05    0.17
Q10   1   0.5756  0.1607 -0.0488  11.00000  0.05    0.16
Q11   1   0.9304  0.2521  0.3065  11.00000  0.05    0.15
Q12   1   1.0525  0.7137  0.2711  11.00000  0.05    0.15
Q13   1   0.9893  0.3881  0.3089  11.00000  0.05    0.14
Q14   1   0.9108  0.3834  0.1164  11.00000  0.05    0.13
Q15   1   0.8934  0.2111  0.1653  11.00000  0.05    0.13
Q16   1   0.8333  0.1667  0.1667  10.50000  0.05    0.13
Q17   1   1.0652  0.6330  0.2794  11.00000  0.05    0.13
Q18   1   0.9417  0.3486  0.3428  11.00000  0.05    0.12
Q19   1   0.4779  0.2193 -0.0520  11.00000  0.05    0.10
Q20   1   0.8333  0.3265  0.2578  11.00000  0.05    0.10
;
_shelx_res_checksum              59763

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c2_p05       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.725 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c2_p05       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.54 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c2_p05       
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.64 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c2_p05       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 63 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT088_DMAFeF_c2_p05       
;
PROBLEM: Poor Data / Parameter Ratio ....................       8.61 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. Additionally,
the positioning of the hydrogen atoms for the dynamically disordered 
(CH3)2NH2 unit could not be performed with standard AFIX commands. Instead
distance restraints are used which increases the number of parameters as the
hydrogen positions are refined.
;
_vrf_PLAT978_DMAFeF_c2_p05       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAFeFc6p03
_database_code_depnum_ccdc_archive 'CCDC 1837763'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Fe4 O24, 4(C2 H8 N)'
_chemical_formula_sum            'C20 H44 Fe4 N4 O24'
_chemical_formula_weight         947.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1967 0.3058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   10.763(11)
_cell_length_b                   8.256(7)
_cell_length_c                   7.985(6)
_cell_angle_alpha                90.26(6)
_cell_angle_beta                 91.72(9)
_cell_angle_gamma                99.47(10)
_cell_volume                     699.5(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    82
_cell_measurement_theta_min      2.2180
_cell_measurement_theta_max      10.9750

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.251
_exptl_crystal_F_000             488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.482
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '7.87 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1769
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.476
_diffrn_reflns_theta_max         12.511
_diffrn_reflns_theta_full        12.511
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measured_fraction_theta_full 0.828
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_Laue_measured_fraction_full 0.828
_diffrn_reflns_point_group_measured_fraction_max 0.559
_diffrn_reflns_point_group_measured_fraction_full 0.559
_reflns_number_total             1769
_reflns_number_gt                827
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.351
_reflns_Friedel_fraction_max     0.291
_reflns_Friedel_fraction_full    0.291

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 4-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.13(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1769
_refine_ls_number_parameters     185
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0790
_refine_ls_wR_factor_ref         0.2059
_refine_ls_wR_factor_gt          0.1867
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.314
_refine_ls_shift/su_mean         0.070

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
Fe1 Fe 0.0328(9) 0.5383(9) 0.4713(9) 0.058(3) Uani 1 1 d . . . . .
Fe2 Fe 0.4885(11) 0.0015(10) 1.0488(10) 0.075(3) Uani 1 1 d . . . . .
Fe3 Fe 0.5052(11) 0.4993(9) 0.5456(10) 0.071(4) Uani 1 1 d . . . . .
Fe4 Fe 0.0136(9) 0.0400(9) 0.9754(10) 0.063(3) Uani 1 1 d D . . . .
O1 O 0.326(4) 0.360(4) 0.647(3) 0.0652(13) Uiso 1 1 d . U . . .
O2 O 0.597(4) 0.108(4) 0.261(4) 0.0652(13) Uiso 1 1 d . U . . .
O3 O 0.128(5) 0.733(4) 0.324(5) 0.0652(13) Uiso 1 1 d . U . . .
O4 O 0.007(4) 0.847(4) 0.787(4) 0.0652(13) Uiso 1 1 d . U . . .
O5 O 0.400(5) 0.816(4) 0.182(5) 0.0652(13) Uiso 1 1 d . U . . .
O6 O 0.426(4) 0.626(4) 0.372(5) 0.0652(13) Uiso 1 1 d . U . . .
O7 O 0.500(4) 0.325(4) 0.366(4) 0.0652(13) Uiso 1 1 d . U . . .
O8 O 0.645(4) -0.132(4) 1.042(4) 0.0652(13) Uiso 1 1 d . U . . .
O9 O 0.499(4) 0.656(3) 0.742(4) 0.0652(13) Uiso 1 1 d . U . . .
O10 O -0.056(4) 0.412(4) 0.267(4) 0.0652(13) Uiso 1 1 d . U . . .
O11 O 0.174(3) 0.183(4) 0.912(3) 0.0652(13) Uiso 1 1 d D U . . .
O12 O 0.175(3) 0.432(4) 0.457(4) 0.0652(13) Uiso 1 1 d . U . . .
O13 O 0.600(4) 0.356(4) 0.707(4) 0.0652(13) Uiso 1 1 d . U . . .
O14 O 0.415(4) 0.875(4) 0.830(5) 0.0652(13) Uiso 1 1 d . U . . .
O15 O 0.116(4) 0.678(4) 0.679(5) 0.0652(13) Uiso 1 1 d . U . . .
O16 O 0.846(4) -0.107(4) 1.036(4) 0.0652(13) Uiso 1 1 d . U . . .
O17 O 0.890(4) 0.656(4) 0.488(4) 0.0652(13) Uiso 1 1 d . U . . .
O18 O 0.030(4) 0.238(4) 0.161(4) 0.0652(13) Uiso 1 1 d . U . . .
O19 O 0.117(4) 0.912(4) 0.137(5) 0.0652(13) Uiso 1 1 d . U . . .
O20 O 0.589(4) 0.228(3) 0.925(4) 0.0652(13) Uiso 1 1 d . U . . .
O21 O -0.082(4) 0.153(4) 0.797(4) 0.0652(13) Uiso 1 1 d . U . . .
O22 O -0.056(4) 0.347(3) 0.589(4) 0.0652(13) Uiso 1 1 d . U . . .
O23 O 0.313(3) 0.109(4) 1.051(4) 0.0652(13) Uiso 1 1 d . U . . .
O24 O 0.679(4) 0.622(4) 0.501(4) 0.0652(13) Uiso 1 1 d . U . . .
C1 C 0.237(6) 0.398(5) 0.577(6) 0.0652(13) Uiso 1 1 d . U . . .
H1 H 0.184520 0.408851 0.665188 0.078 Uiso 1 1 calc R U . . .
C2 C 0.752(7) -0.034(7) 1.029(8) 0.0652(13) Uiso 1 1 d . U . . .
H2 H 0.758474 0.078912 1.015509 0.078 Uiso 1 1 calc R U . . .
C3 C 0.116(5) 0.804(5) 0.775(6) 0.0652(13) Uiso 1 1 d . U . . .
H3 H 0.188050 0.857784 0.831200 0.078 Uiso 1 1 calc R U . . .
C4 C 0.116(5) 0.061(6) 0.489(7) 0.0652(13) Uiso 1 1 d D U . . .
H4A H 0.061759 0.132741 0.444086 0.078 Uiso 1 1 calc R U . . .
H4B H 0.078815 -0.050952 0.466455 0.078 Uiso 1 1 calc R U . . .
H4C H 0.127513 0.078649 0.607543 0.078 Uiso 1 1 calc R U . . .
C5 C 0.443(6) 0.743(6) 0.310(6) 0.0652(13) Uiso 1 1 d . U . . .
H5 H 0.508731 0.813125 0.365223 0.078 Uiso 1 1 calc R U . . .
C6 C 0.178(5) 0.539(6) 0.022(6) 0.0652(13) Uiso 1 1 d D U . . .
H6A H 0.105615 0.538304 0.088424 0.078 Uiso 1 1 calc R U . . .
H6B H 0.213405 0.650283 -0.004615 0.078 Uiso 1 1 calc R U . . .
H6C H 0.154405 0.478254 -0.080266 0.078 Uiso 1 1 calc R U . . .
C7 C 0.566(5) 0.225(6) 0.352(7) 0.0652(13) Uiso 1 1 d . U . . .
H7 H 0.617963 0.233366 0.447083 0.078 Uiso 1 1 calc R U . . .
C8 C 0.434(5) 0.758(6) 0.752(6) 0.0652(13) Uiso 1 1 d . U . . .
H8 H 0.373661 0.738618 0.665804 0.078 Uiso 1 1 calc R U . . .
C9 C 0.273(6) 0.124(5) 0.898(5) 0.0652(13) Uiso 1 1 d . U . . .
H9 H 0.309746 0.096105 0.800297 0.078 Uiso 1 1 calc R U . . .
C10 C 0.697(4) 1.018(4) 0.627(5) 0.0652(13) Uiso 1 1 d D U . . .
H10A H 0.688863 0.993115 0.744416 0.078 Uiso 1 1 calc R U . . .
H10B H 0.713969 1.134484 0.613181 0.078 Uiso 1 1 calc R U . . .
H10C H 0.619250 0.973708 0.568395 0.078 Uiso 1 1 calc R U . . .
C11 C 0.569(6) 0.227(6) 0.777(6) 0.0652(13) Uiso 1 1 d . U . . .
H11 H 0.531278 0.132570 0.719478 0.078 Uiso 1 1 calc R U . . .
C12 C -0.077(6) 0.295(6) 0.178(6) 0.0652(13) Uiso 1 1 d . U . . .
H12 H -0.154696 0.250709 0.128438 0.078 Uiso 1 1 calc R U . . .
C13 C 0.690(6) 0.547(5) 1.111(4) 0.0652(13) Uiso 1 1 d D U . . .
H13A H 0.602165 0.530079 1.134988 0.078 Uiso 1 1 calc R U . . .
H13B H 0.726259 0.454111 1.149436 0.078 Uiso 1 1 calc R U . . .
H13C H 0.732194 0.644441 1.167176 0.078 Uiso 1 1 calc R U . . .
C14 C 0.056(6) 0.772(6) 0.230(5) 0.0652(13) Uiso 1 1 d . U . . .
H13 H -0.027581 0.721515 0.215317 0.078 Uiso 1 1 calc R U . . .
C15 C -0.030(6) 0.285(6) 0.730(6) 0.0652(13) Uiso 1 1 d . U . . .
H15 H 0.036238 0.345612 0.791700 0.078 Uiso 1 1 calc R U . . .
C16 C 0.393(5) 0.452(6) 0.034(7) 0.0652(13) Uiso 1 1 d D U . . .
H16A H 0.445207 0.400350 0.108867 0.078 Uiso 1 1 calc R U . . .
H16B H 0.376558 0.388393 -0.067795 0.078 Uiso 1 1 calc R U . . .
H16C H 0.435559 0.560422 0.007855 0.078 Uiso 1 1 calc R U . . .
C17 C 0.308(5) -0.021(5) 0.490(6) 0.0652(13) Uiso 1 1 d D U . . .
H17A H 0.391559 -0.008929 0.447330 0.078 Uiso 1 1 calc R U . . .
H17B H 0.313786 -0.001215 0.609236 0.078 Uiso 1 1 calc R U . . .
H17C H 0.265088 -0.130816 0.468148 0.078 Uiso 1 1 calc R U . . .
C18 C 0.816(6) 0.979(5) 0.377(4) 0.0652(13) Uiso 1 1 d D U . . .
H18A H 0.882375 0.932578 0.327820 0.078 Uiso 1 1 calc R U . . .
H18B H 0.737028 0.935356 0.320468 0.078 Uiso 1 1 calc R U . . .
H18C H 0.831747 1.096131 0.365254 0.078 Uiso 1 1 calc R U . . .
C19 C 0.779(8) 0.578(8) 0.488(8) 0.0652(13) Uiso 1 1 d . U . . .
H19 H 0.774128 0.465082 0.476534 0.078 Uiso 1 1 calc R U . . .
C20 C 0.834(4) 0.589(4) 0.892(5) 0.0652(13) Uiso 1 1 d D U . . .
H20A H 0.836606 0.598798 0.772643 0.078 Uiso 1 1 calc R U . . .
H20B H 0.878533 0.687069 0.944245 0.078 Uiso 1 1 calc R U . . .
H20C H 0.872598 0.496739 0.926505 0.078 Uiso 1 1 calc R U . . .
N1 N 0.704(4) 0.563(4) 0.942(4) 0.0652(13) Uiso 1 1 d D U . . .
H21A H 0.668772 0.647256 0.907628 0.078 Uiso 1 1 calc R U . . .
H21B H 0.663332 0.472821 0.891370 0.078 Uiso 1 1 calc R U . . .
N2 N 0.239(4) 0.096(4) 0.409(5) 0.0652(13) Uiso 1 1 d D U . . .
H22A H 0.231069 0.079396 0.299212 0.078 Uiso 1 1 calc R U . . .
H22B H 0.276142 0.199350 0.429798 0.078 Uiso 1 1 calc R U . . .
N3 N 0.272(4) 0.464(4) 0.114(5) 0.0652(13) Uiso 1 1 d D U . . .
H23A H 0.235746 0.363000 0.140680 0.078 Uiso 1 1 calc R U . . .
H23B H 0.289621 0.520086 0.209759 0.078 Uiso 1 1 calc R U . . .
N4 N 0.809(4) 0.937(4) 0.555(4) 0.0652(13) Uiso 1 1 d D U . . .
H24A H 0.881172 0.976965 0.608375 0.078 Uiso 1 1 calc R U . . .
H24B H 0.793835 0.828721 0.567080 0.078 Uiso 1 1 calc R U . . .

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
Fe1 0.057(8) 0.059(5) 0.056(6) 0.005(4) -0.003(5) 0.005(6)
Fe2 0.102(10) 0.081(6) 0.041(5) -0.005(4) -0.010(6) 0.017(7)
Fe3 0.103(11) 0.065(6) 0.050(5) -0.010(4) -0.004(6) 0.031(6)
Fe4 0.072(9) 0.061(5) 0.050(5) 0.011(4) -0.003(6) -0.006(6)

_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
Fe1 O12 1.89(3) . ?
Fe1 O17 1.96(4) 1_455 ?
Fe1 O22 1.97(3) . ?
Fe1 O10 2.05(4) . ?
Fe1 O15 2.10(4) . ?
Fe1 O3 2.14(4) . ?
Fe2 O5 1.99(4) 1_546 ?
Fe2 O14 2.10(4) 1_545 ?
Fe2 O2 2.13(4) 1_556 ?
Fe2 O8 2.16(4) . ?
Fe2 O23 2.22(3) . ?
Fe2 O20 2.25(3) . ?
Fe3 O6 1.99(4) . ?
Fe3 O7 2.02(3) . ?
Fe3 O24 2.02(4) . ?
Fe3 O9 2.04(4) . ?
Fe3 O13 2.11(4) . ?
Fe3 O1 2.25(3) . ?
Fe4 O11 2.01(3) . ?
Fe4 O21 2.05(4) . ?
Fe4 O16 2.07(4) 1_455 ?
Fe4 O19 2.08(4) 1_546 ?
Fe4 O4 2.18(3) 1_545 ?
Fe4 O18 2.18(3) 1_556 ?
O1 C1 1.18(6) . ?
O2 C7 1.30(6) . ?
O3 C14 1.15(6) . ?
O4 C3 1.29(6) . ?
O5 C5 1.31(6) . ?
O6 C5 1.08(5) . ?
O7 C7 1.18(6) . ?
O8 C2 1.31(7) . ?
O9 C8 1.18(6) . ?
O10 C12 1.19(5) . ?
O11 C9 1.26(7) . ?
O12 C1 1.22(5) . ?
O13 C11 1.21(6) . ?
O14 C8 1.20(5) . ?
O15 C3 1.29(5) . ?
O16 C2 1.26(7) . ?
O17 C19 1.26(8) . ?
O18 C12 1.32(7) . ?
O19 C14 1.45(6) . ?
O20 C11 1.19(6) . ?
O21 C15 1.27(5) . ?
O22 C15 1.28(6) . ?
O23 C9 1.29(5) . ?
O24 C19 1.20(8) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 N2 1.47(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5 0.9300 . ?
C6 N3 1.45(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 N4 1.59(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 N1 1.36(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H13 0.9300 . ?
C15 H15 0.9300 . ?
C16 N3 1.49(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N2 1.46(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N4 1.46(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9300 . ?
C20 N1 1.44(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
N1 H21A 0.8900 . ?
N1 H21B 0.8900 . ?
N2 H22A 0.8900 . ?
N2 H22B 0.8900 . ?
N3 H23A 0.8900 . ?
N3 H23B 0.8900 . ?
N4 H24A 0.8900 . ?
N4 H24B 0.8900 . ?

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
O12 Fe1 O17 177.9(18) . 1_455 ?
O12 Fe1 O22 89.6(16) . . ?
O17 Fe1 O22 92.1(17) 1_455 . ?
O12 Fe1 O10 92.4(14) . . ?
O17 Fe1 O10 89.2(15) 1_455 . ?
O22 Fe1 O10 81.5(14) . . ?
O12 Fe1 O15 90.8(16) . . ?
O17 Fe1 O15 87.6(16) 1_455 . ?
O22 Fe1 O15 99.5(14) . . ?
O10 Fe1 O15 176.6(16) . . ?
O12 Fe1 O3 88.8(17) . . ?
O17 Fe1 O3 89.8(17) 1_455 . ?
O22 Fe1 O3 174.9(15) . . ?
O10 Fe1 O3 93.8(16) . . ?
O15 Fe1 O3 85.3(15) . . ?
O5 Fe2 O14 88.7(15) 1_546 1_545 ?
O5 Fe2 O2 92.8(16) 1_546 1_556 ?
O14 Fe2 O2 168.0(17) 1_545 1_556 ?
O5 Fe2 O8 87.0(18) 1_546 . ?
O14 Fe2 O8 88.1(16) 1_545 . ?
O2 Fe2 O8 80.1(13) 1_556 . ?
O5 Fe2 O23 87.7(18) 1_546 . ?
O14 Fe2 O23 87.1(15) 1_545 . ?
O2 Fe2 O23 104.8(13) 1_556 . ?
O8 Fe2 O23 172.9(16) . . ?
O5 Fe2 O20 173.5(15) 1_546 . ?
O14 Fe2 O20 97.3(13) 1_545 . ?
O2 Fe2 O20 81.8(14) 1_556 . ?
O8 Fe2 O20 95.7(16) . . ?
O23 Fe2 O20 90.1(15) . . ?
O6 Fe3 O7 85.8(16) . . ?
O6 Fe3 O24 92.0(15) . . ?
O7 Fe3 O24 97.3(18) . . ?
O6 Fe3 O9 97.6(14) . . ?
O7 Fe3 O9 173.7(17) . . ?
O24 Fe3 O9 87.9(16) . . ?
O6 Fe3 O13 173.5(15) . . ?
O7 Fe3 O13 89.0(14) . . ?
O24 Fe3 O13 84.9(15) . . ?
O9 Fe3 O13 87.9(13) . . ?
O6 Fe3 O1 97.5(16) . . ?
O7 Fe3 O1 89.3(14) . . ?
O24 Fe3 O1 168.9(13) . . ?
O9 Fe3 O1 85.1(13) . . ?
O13 Fe3 O1 86.3(15) . . ?
O11 Fe4 O21 89.1(15) . . ?
O11 Fe4 O16 178.8(14) . 1_455 ?
O21 Fe4 O16 89.7(15) . 1_455 ?
O11 Fe4 O19 89.6(16) . 1_546 ?
O21 Fe4 O19 174.0(14) . 1_546 ?
O16 Fe4 O19 91.6(15) 1_455 1_546 ?
O11 Fe4 O4 99.1(14) . 1_545 ?
O21 Fe4 O4 84.4(13) . 1_545 ?
O16 Fe4 O4 80.4(14) 1_455 1_545 ?
O19 Fe4 O4 90.0(13) 1_546 1_545 ?
O11 Fe4 O18 78.1(15) . 1_556 ?
O21 Fe4 O18 96.0(14) . 1_556 ?
O16 Fe4 O18 102.5(17) 1_455 1_556 ?
O19 Fe4 O18 89.5(15) 1_546 1_556 ?
O4 Fe4 O18 177(2) 1_545 1_556 ?
C1 O1 Fe3 110(3) . . ?
C7 O2 Fe2 123(4) . 1_554 ?
C14 O3 Fe1 108(4) . . ?
C3 O4 Fe4 111(3) . 1_565 ?
C5 O5 Fe2 128(4) . 1_564 ?
C5 O6 Fe3 140(5) . . ?
C7 O7 Fe3 129(4) . . ?
C2 O8 Fe2 112(4) . . ?
C8 O9 Fe3 127(4) . . ?
C12 O10 Fe1 152(3) . . ?
C9 O11 Fe4 120(3) . . ?
C1 O12 Fe1 124(3) . . ?
C11 O13 Fe3 133(4) . . ?
C8 O14 Fe2 137(4) . 1_565 ?
C3 O15 Fe1 147(4) . . ?
C2 O16 Fe4 114(3) . 1_655 ?
C19 O17 Fe1 120(4) . 1_655 ?
C12 O18 Fe4 113(3) . 1_554 ?
C14 O19 Fe4 121(4) . 1_564 ?
C11 O20 Fe2 112(3) . . ?
C15 O21 Fe4 121(4) . . ?
C15 O22 Fe1 130(4) . . ?
C9 O23 Fe2 109(3) . . ?
C19 O24 Fe3 133(4) . . ?
O1 C1 O12 156(6) . . ?
O1 C1 H1 102.1 . . ?
O12 C1 H1 102.1 . . ?
O16 C2 O8 113(5) . . ?
O16 C2 H2 123.2 . . ?
O8 C2 H2 123.4 . . ?
O4 C3 O15 114(4) . . ?
O4 C3 H3 123.2 . . ?
O15 C3 H3 122.8 . . ?
N2 C4 H4A 109.6 . . ?
N2 C4 H4B 109.9 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.0 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O6 C5 O5 139(7) . . ?
O6 C5 H5 110.5 . . ?
O5 C5 H5 110.7 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O7 C7 O2 148(6) . . ?
O7 C7 H7 106.3 . . ?
O2 C7 H7 106.1 . . ?
O9 C8 O14 145(6) . . ?
O9 C8 H8 107.3 . . ?
O14 C8 H8 107.6 . . ?
O11 C9 O23 104(4) . . ?
O11 C9 H9 127.9 . . ?
O23 C9 H9 127.7 . . ?
N4 C10 H10A 109.6 . . ?
N4 C10 H10B 109.4 . . ?
H10A C10 H10B 109.5 . . ?
N4 C10 H10C 109.4 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O20 C11 O13 116(5) . . ?
O20 C11 H11 122.2 . . ?
O13 C11 H11 122.1 . . ?
O10 C12 O18 108(5) . . ?
O10 C12 H12 126.1 . . ?
O18 C12 H12 126.1 . . ?
N1 C13 H13A 109.3 . . ?
N1 C13 H13B 109.6 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O3 C14 O19 109(5) . . ?
O3 C14 H13 125.6 . . ?
O19 C14 H13 125.6 . . ?
O21 C15 O22 129(6) . . ?
O21 C15 H15 115.3 . . ?
O22 C15 H15 115.5 . . ?
N3 C16 H16A 109.2 . . ?
N3 C16 H16B 110.0 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.3 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 H17A 109.2 . . ?
N2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N2 C17 H17C 109.6 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.3 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.6 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O24 C19 O17 132(6) . . ?
O24 C19 H19 114.0 . . ?
O17 C19 H19 113.8 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C13 N1 C20 114(4) . . ?
C13 N1 H21A 108.8 . . ?
C20 N1 H21A 108.7 . . ?
C13 N1 H21B 108.8 . . ?
C20 N1 H21B 108.7 . . ?
H21A N1 H21B 107.6 . . ?
C17 N2 C4 102(4) . . ?
C17 N2 H22A 111.4 . . ?
C4 N2 H22A 110.8 . . ?
C17 N2 H22B 111.5 . . ?
C4 N2 H22B 111.7 . . ?
H22A N2 H22B 109.2 . . ?
C6 N3 C16 119(4) . . ?
C6 N3 H23A 107.6 . . ?
C16 N3 H23A 107.4 . . ?
C6 N3 H23B 107.6 . . ?
C16 N3 H23B 108.1 . . ?
H23A N3 H23B 107.0 . . ?
C18 N4 C10 107(3) . . ?
C18 N4 H24A 110.2 . . ?
C10 N4 H24A 110.3 . . ?
C18 N4 H24B 110.6 . . ?
C10 N4 H24B 110.4 . . ?
H24A N4 H24B 108.6 . . ?

_refine_diff_density_max         0.889
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.170

_shelx_res_file                  
;
REM SHELXT solution in P1
REM R1 0.377,  Rweak 0.093,  Alpha 0.000,  Orientation as input
REM Flack x = -0.469 ( 0.801 ) from Parsons' quotients
REM Formula found by SHELXT:

CELL  0.41119  10.7631   8.2558   7.9845   90.263   91.718   99.468
ZERR    4.000   0.0114   0.0071   0.0057    0.063    0.093    0.103
LATT -1
SFAC C H N O FE
DISP $C -0.00006  0.00048  5.14212!source kissel
DISP $H -0.00003  0.00000  0.64130!source kissel
DISP $N  0.00062  0.00099  7.19266!source kissel
DISP $O  0.00180  0.00183 10.15895!source kissel
DISP $Fe  0.19674  0.30575 741.22085!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00

OMIT 7 -5 5
OMIT -6 -1 3
OMIT 7 -3 3
OMIT 7 -5 3
OMIT 6  -1   1
OMIT -6   0  -1
L.S. 50
ACTA
BOND $H
LIST 4
FMAP 2
PLAN 20
MERG 0
WGHT    0.100000
BASF   0.14881   0.29627   0.23687
FVAR       6.46285   0.06516
FE1   5    0.032762    0.538330    0.471311    11.00000    0.05654    0.05897 =
         0.05565    0.00457   -0.00300    0.00511
FE2   5    0.488501    0.001518    1.048796    11.00000    0.10153    0.08131 =
         0.04136   -0.00513   -0.00998    0.01709
FE3   5    0.505226    0.499281    0.545584    11.00000    0.10294    0.06509 =
         0.04973   -0.01048   -0.00400    0.03094
FE4   5    0.013583    0.040022    0.975427    11.00000    0.07237    0.06082 =
         0.04985    0.01077   -0.00267   -0.00603
DFIX Fe4 O11 2.0 0.05
O1    4    0.325801    0.359728    0.647145    11.00000   21.00000
O2    4    0.596994    0.108048    0.261058    11.00000   21.00000
O3    4    0.127885    0.733165    0.324262    11.00000   21.00000
O4    4    0.007065    0.847363    0.786611    11.00000   21.00000
O5    4    0.399765    0.816204    0.181852    11.00000   21.00000
O6    4    0.426182    0.625796    0.371923    11.00000   21.00000
O7    4    0.499778    0.324971    0.366429    11.00000   21.00000
O8    4    0.644609   -0.132266    1.042011    11.00000   21.00000
O9    4    0.499451    0.656108    0.741782    11.00000   21.00000
O10   4   -0.055775    0.412414    0.267480    11.00000   21.00000
O11   4    0.173817    0.183484    0.911881    11.00000   21.00000
O12   4    0.175041    0.431840    0.456596    11.00000   21.00000
O13   4    0.600356    0.356290    0.707179    11.00000   21.00000
O14   4    0.415284    0.875037    0.829536    11.00000   21.00000
O15   4    0.116191    0.677580    0.678783    11.00000   21.00000
O16   4    0.846006   -0.107274    1.036266    11.00000   21.00000
O17   4    0.889800    0.656164    0.488488    11.00000   21.00000
O18   4    0.029502    0.237683    0.160531    11.00000   21.00000
O19   4    0.116869    0.911532    0.136928    11.00000   21.00000
O20   4    0.588642    0.228485    0.924734    11.00000   21.00000
O21   4   -0.081634    0.152562    0.796609    11.00000   21.00000
O22   4   -0.056369    0.346595    0.588812    11.00000   21.00000
O23   4    0.312718    0.109379    1.050577    11.00000   21.00000
O24   4    0.679069    0.621899    0.500567    11.00000   21.00000
C1    1    0.237346    0.398112    0.577179    11.00000   21.00000
AFIX  43
H1    2    0.184520    0.408851    0.665188    11.00000   -1.20000
AFIX   0
C2    1    0.751949   -0.033981    1.028922    11.00000   21.00000
AFIX  43
H2    2    0.758474    0.078912    1.015509    11.00000   -1.20000
AFIX   0
C3    1    0.116027    0.803556    0.775137    11.00000   21.00000
AFIX  43
H3    2    0.188050    0.857784    0.831200    11.00000   -1.20000
AFIX   0
C4    1    0.116108    0.061171    0.488742    11.00000   21.00000
AFIX  33
H4A   2    0.061759    0.132741    0.444086    11.00000   -1.20000
H4B   2    0.078815   -0.050952    0.466455    11.00000   -1.20000
H4C   2    0.127513    0.078649    0.607543    11.00000   -1.20000
AFIX   0
C5    1    0.443410    0.743173    0.310423    11.00000   21.00000
AFIX  43
H5    2    0.508731    0.813125    0.365223    11.00000   -1.20000
AFIX   0
C6    1    0.178396    0.539068    0.021624    11.00000   21.00000
AFIX  33
H6A   2    0.105615    0.538304    0.088424    11.00000   -1.20000
H6B   2    0.213405    0.650283   -0.004615    11.00000   -1.20000
H6C   2    0.154405    0.478254   -0.080266    11.00000   -1.20000
AFIX   0
C7    1    0.565586    0.224690    0.351574    11.00000   21.00000
AFIX  43
H7    2    0.617963    0.233366    0.447083    11.00000   -1.20000
AFIX   0
C8    1    0.434307    0.757631    0.752203    11.00000   21.00000
AFIX  43
H8    2    0.373661    0.738618    0.665804    11.00000   -1.20000
AFIX   0
C9    1    0.273093    0.123739    0.898175    11.00000   21.00000
AFIX  43
H9    2    0.309746    0.096105    0.800297    11.00000   -1.20000
AFIX   0
C10   1    0.696568    1.017623    0.627401    11.00000   21.00000
AFIX  33
H10A  2    0.688863    0.993115    0.744416    11.00000   -1.20000
H10B  2    0.713969    1.134484    0.613181    11.00000   -1.20000
H10C  2    0.619250    0.973708    0.568395    11.00000   -1.20000
AFIX   0
C11   1    0.568729    0.227001    0.777207    11.00000   21.00000
AFIX  43
H11   2    0.531278    0.132570    0.719478    11.00000   -1.20000
AFIX   0
C12   1   -0.076954    0.294584    0.177632    11.00000   21.00000
AFIX  43
H12   2   -0.154696    0.250709    0.128438    11.00000   -1.20000
AFIX   0
C13   1    0.690193    0.546678    1.110980    11.00000   21.00000
AFIX  33
H13A  2    0.602165    0.530079    1.134988    11.00000   -1.20000
H13B  2    0.726259    0.454111    1.149436    11.00000   -1.20000
H13C  2    0.732194    0.644441    1.167176    11.00000   -1.20000
AFIX   0
C14   1    0.055987    0.771720    0.229832    11.00000   21.00000
AFIX  43
H13   2   -0.027581    0.721515    0.215317    11.00000   -1.20000
AFIX   0
C15   1   -0.030061    0.284897    0.729631    11.00000   21.00000
AFIX  43
H15   2    0.036238    0.345612    0.791700    11.00000   -1.20000
AFIX   0
C16   1    0.393046    0.452279    0.033586    11.00000   21.00000
AFIX  33
H16A  2    0.445207    0.400350    0.108867    11.00000   -1.20000
H16B  2    0.376558    0.388393   -0.067795    11.00000   -1.20000
H16C  2    0.435559    0.560422    0.007855    11.00000   -1.20000
AFIX   0
C17   1    0.308272   -0.021230    0.490499    11.00000   21.00000
AFIX  33
H17A  2    0.391559   -0.008929    0.447330    11.00000   -1.20000
H17B  2    0.313786   -0.001215    0.609236    11.00000   -1.20000
H17C  2    0.265088   -0.130816    0.468148    11.00000   -1.20000
AFIX   0
C18   1    0.815579    0.978910    0.376728    11.00000   21.00000
AFIX  33
H18A  2    0.882375    0.932578    0.327820    11.00000   -1.20000
H18B  2    0.737028    0.935356    0.320468    11.00000   -1.20000
H18C  2    0.831747    1.096131    0.365254    11.00000   -1.20000
AFIX   0
C19   1    0.779203    0.578120    0.488349    11.00000   21.00000
AFIX  43
H19   2    0.774128    0.465082    0.476534    11.00000   -1.20000
AFIX   0
C20   1    0.833880    0.588520    0.892244    11.00000   21.00000
AFIX  33
H20A  2    0.836606    0.598798    0.772643    11.00000   -1.20000
H20B  2    0.878533    0.687069    0.944245    11.00000   -1.20000
H20C  2    0.872598    0.496739    0.926505    11.00000   -1.20000
AFIX   0
N1    3    0.704341    0.562876    0.942406    11.00000   21.00000
AFIX  23
H21A  2    0.668772    0.647256    0.907628    11.00000   -1.20000
H21B  2    0.663332    0.472821    0.891370    11.00000   -1.20000
AFIX   0
N2    3    0.238797    0.096452    0.409449    11.00000   21.00000
AFIX  23
H22A  2    0.231069    0.079396    0.299212    11.00000   -1.20000
H22B  2    0.276142    0.199350    0.429798    11.00000   -1.20000
AFIX   0
N3    3    0.271550    0.464201    0.114126    11.00000   21.00000
AFIX  23
H23A  2    0.235746    0.363000    0.140680    11.00000   -1.20000
H23B  2    0.289621    0.520086    0.209759    11.00000   -1.20000
AFIX   0
N4    3    0.808845    0.937199    0.554696    11.00000   21.00000
AFIX  23
H24A  2    0.881172    0.976965    0.608375    11.00000   -1.20000
H24B  2    0.793835    0.828721    0.567080    11.00000   -1.20000
DFIX N1 C20 1.4 0.05
DFIX N1 C13 1.4 0.05
DANG 2.4 0.2 C13 C20
DFIX N2 C17 1.4 0.05
DFIX N2 C4 1.4 0.05
DANG 2.4 0.2 C4 C17
DFIX N3 C16 1.4 0.05
DFIX N3 C6 1.4 0.05
DANG 2.4 0.2 C16 C6
DFIX N4 C10 1.4 0.05
DFIX N4 C18 1.4 0.05
DANG 2.4 0.2 C10 C18
AFIX   0
HKLF 5




REM
REM R1 =  0.0790 for     827 Fo > 4sig(Fo)  and  0.1347 for all    1769 data
REM    185 parameters refined using     16 restraints

END

WGHT      0.1401      0.0000

REM Highest difference peak  0.889,  deepest hole -0.657,  1-sigma level  0.170
Q1    1   0.5571  0.1062  0.8906  11.00000  0.05    0.89
Q2    1  -0.0452  0.4443  0.6378  11.00000  0.05    0.86
Q3    1   0.0468  0.1016  0.9620  11.00000  0.05    0.76
Q4    1   0.5268 -0.0665  0.9697  11.00000  0.05    0.76
Q5    1   0.0705  0.5833  0.4539  11.00000  0.05    0.74
Q6    1   0.5195  0.6088  0.4306  11.00000  0.05    0.72
Q7    1   0.5429  0.4109  0.4763  11.00000  0.05    0.70
Q8    1  -0.0592  0.0752  0.9376  11.00000  0.05    0.69
Q9    1   0.4474 -0.0480  1.0720  11.00000  0.05    0.69
Q10   1   0.1209  0.9875 -0.0035  11.00000  0.05    0.65
Q11   1   0.5994 -0.0622  1.0689  11.00000  0.05    0.65
Q12   1   0.0922  0.5296  0.5306  11.00000  0.05    0.64
Q13   1   0.4029  0.5553  0.5365  11.00000  0.05    0.60
Q14   1  -0.0009  0.6310  0.5600  11.00000  0.05    0.60
Q15   1   0.0034 -0.0606  1.0965  11.00000  0.05    0.60
Q16   1   0.0962  0.0109  1.0309  11.00000  0.05    0.59
Q17   1   0.9429  0.5957  0.4332  11.00000  0.05    0.58
Q18   1   0.9030  0.5846  0.4666  11.00000  0.05    0.58
Q19   1   0.4628  0.4144  0.5755  11.00000  0.05    0.58
Q20   1  -0.0234  0.0276  0.9908  11.00000  0.05    0.56
;
_shelx_res_checksum              43414


# start Validation Reply Form
_vrf_SHFSU01_DMAFeFc6p03         
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: Refinement was carried out several times with 50 cycles, however,
due to the many parameters and the limited diffraction data available, this
does not allow a complete convergence of the refinement.
;
_vrf_THETM01_DMAFeFc6p03         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The resolution of the data was significantly reduced upon the
phase transition and therefore integration was carried out up to 0.95 
Angstrom.
;
_vrf_PLAT111_DMAFeFc6p03         
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit 
RESPONSE: P-1 symmetry was tested for structure solution, however, a suitable
structure could not be refined. If the P-1 symmetry is used, it would result in
additional occupational disorder of the formate ligands (as observed in the 
high-pressure DMACuF phase). As the unit cell is quite large, and there are a
significant number of atoms in the unit cell, this structural disorder 
is not trivial to implement. 
;
_vrf_PLAT113_DMAFeFc6p03         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group        P-1 Check 
RESPONSE: P-1 symmetry was tested for structure solution, however, a suitable
structure could not be refined. If the P-1 symmetry is used, it would result in
additional occupational disorder of the formate ligands (as observed in the 
high-pressure DMACuF phase). As the unit cell is quite large, and there are a
significant number of atoms in the unit cell, this structural disorder 
is not trivial to implement.  
;
_vrf_PLAT911_DMAFeFc6p03         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.527 509 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_REFNR01_DMAFeFc6p03         
;
PROBLEM: Ratio of reflections to parameters is < 10 for a
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. In addition,
there are many atoms in the unit cell and there is a loss of resolution
in the diffraction data upon the transition, giving rise to the poor data/
parameter ratio.
;
_vrf_PLAT029_DMAFeFc6p03         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.828 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT080_DMAFeFc6p03         
;
PROBLEM: Maximum Shift/Error ............................       0.31 Why ? 
RESPONSE: Refinement was carried out several times with 50 cycles, however,
due to the many parameters and the limited diffraction data available, this
does not allow a complete convergence of the refinement.
;
_vrf_PLAT201_DMAFeFc6p03         
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         36 Report
RESPONSE: Due to the many parameters in the refinement, refinement
of isotropic thermal parameters were preferred.
;
_vrf_PLAT411_DMAFeFc6p03         
;
PROBLEM: Short Inter H...H Contact  H2       ..H12              1.79 Ang.  
RESPONSE: Due to the large distortions in the framework in this high
pressure phase, certain H...H contacts are short. Additionally, the 
positioning of the H atoms are through the AFIX commands, and may not 
be optimised for the high-pressure conditions.
;
_vrf_PLAT413_DMAFeFc6p03         
;
PROBLEM: Short Inter XH3 .. XHn     H9       ..H17B             1.73 Ang.  
RESPONSE: Due to the large distortions in the framework in this high
pressure phase, certain H...H contacts are short. Additionally, the 
positioning of the H atoms are through the AFIX commands, and may not 
be optimised for the high-pressure conditions.
;
_vrf_PLAT026_DMAFeFc6p03         
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        47% Check 
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT090_DMAFeFc6p03         
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       6.52 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. In addition,
there are many atoms in the unit cell and there is a loss of resolution
in the diffraction data upon the transition, giving rise to the poor data/
parameter ratio.
;
_vrf_PLAT148_DMAFeFc6p03         
;
PROBLEM: s.u. on the      a    - Axis is (Too) Large ....      0.011 Ang.  
RESPONSE: The diffraction spots are broader giving rise to larger errors
in the unit cell parameters.
;
_vrf_PLAT155_DMAFeFc6p03         
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do ! 
RESPONSE: The cell was kept in the given setting so as to be more
comparable to the ambient phase unit cell.
;
_vrf_PLAT202_DMAFeFc6p03         
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........         12 Check 
RESPONSE: Due to the many parameters in the refinement, refinement
of isotropic thermal parameters were preferred.
;
_vrf_PLAT410_DMAFeFc6p03         
;
PROBLEM: Short Intra H...H Contact  H1       ..H15              1.92 Ang.  
RESPONSE: Due to the large distortions in the framework in this high
pressure phase, certain H...H contacts are short. Additionally, the 
positioning of the H atoms are through the AFIX commands, and may not 
be optimised for the high-pressure conditions.
;
_vrf_PLAT906_DMAFeFc6p03         
;
PROBLEM: Large K Value in the Analysis of Variance ......      3.286 Check 
RESPONSE: The large K value is only observed at the highest resolution
where the weakest reflections are observed.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_DMAFeF_c2_p04
_database_code_depnum_ccdc_archive 'CCDC 1837758'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.0225(6)
_cell_length_b                   8.0225(6)
_cell_length_c                   21.1076(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1176.49(19)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    175
_cell_measurement_theta_min      2.9390
_cell_measurement_theta_max      14.7640

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.429
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89885
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '3.94 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            748
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.937
_diffrn_reflns_theta_max         19.349
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.466
_diffrn_measured_fraction_theta_full 0.731
_diffrn_reflns_Laue_measured_fraction_max 0.466
_diffrn_reflns_Laue_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.466
_diffrn_reflns_point_group_measured_fraction_full 0.731
_reflns_number_total             270
_reflns_number_gt                214
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0470P)²+6.9966P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         270
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1165
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0368(5) Uani 1 6 d S T P . .
N1 N 0.745(2) 0.333333 0.083333 0.061(5) Uani 0.3333 2 d DS T P . .
H3 H 0.781(10) 0.245(10) 0.091(10) 0.073 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0263(5) 0.073(3) Uani 1 3 d DS T P . .
H2 H 0.544(6) 0.252(8) -0.006(3) 0.087 Uiso 1 1 d D U . . .
O1 O 0.8671(5) 0.3060(5) 0.27780(15) 0.0495(9) Uani 1 1 d . . . . .
C1 C 1.000000 0.4437(8) 0.250000 0.0422(12) Uani 1 2 d S T P . .
H1 H 1.000001 0.559636 0.250000 0.051 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0386(7) 0.0386(7) 0.0332(8) 0.000 0.000 0.0193(3)
N1 0.052(7) 0.045(9) 0.082(17) -0.010(10) -0.005(5) 0.022(4)
C2 0.090(5) 0.090(5) 0.038(6) 0.000 0.000 0.045(3)
O1 0.0513(19) 0.0462(18) 0.0522(19) 0.0050(13) 0.0137(14) 0.0253(15)
C1 0.043(3) 0.041(2) 0.043(3) 0.0008(11) 0.002(2) 0.0214(16)

_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
Fe1 O1 2.088(3) 31_655 ?
Fe1 O1 2.088(3) 33_545 ?
Fe1 O1 2.088(3) . ?
Fe1 O1 2.088(3) 3_665 ?
Fe1 O1 2.088(3) 32 ?
Fe1 O1 2.088(3) 2_655 ?
N1 N1 1.09(3) 3_665 ?
N1 N1 1.09(3) 2_655 ?
N1 C2 1.359(13) 16_544 ?
N1 C2 1.359(13) . ?
O1 C1 1.234(4) . ?

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 Fe1 O1 91.57(13) 31_655 33_545 ?
O1 Fe1 O1 180.0 31_655 . ?
O1 Fe1 O1 88.43(13) 33_545 . ?
O1 Fe1 O1 88.43(13) 31_655 3_665 ?
O1 Fe1 O1 180.0 33_545 3_665 ?
O1 Fe1 O1 91.57(13) . 3_665 ?
O1 Fe1 O1 91.57(13) 31_655 32 ?
O1 Fe1 O1 91.57(13) 33_545 32 ?
O1 Fe1 O1 88.43(13) . 32 ?
O1 Fe1 O1 88.43(13) 3_665 32 ?
O1 Fe1 O1 88.43(13) 31_655 2_655 ?
O1 Fe1 O1 88.43(13) 33_545 2_655 ?
O1 Fe1 O1 91.57(13) . 2_655 ?
O1 Fe1 O1 91.57(13) 3_665 2_655 ?
O1 Fe1 O1 180.0 32 2_655 ?
N1 N1 N1 59.998(1) 3_665 2_655 ?
N1 N1 C2 66.3(6) 3_665 16_544 ?
N1 N1 C2 66.3(6) 2_655 16_544 ?
N1 N1 C2 66.3(6) 3_665 . ?
N1 N1 C2 66.3(6) 2_655 . ?
C2 N1 C2 124.8(14) 16_544 . ?
N1 C2 N1 47.3(12) . 3_665 ?
N1 C2 N1 47.3(12) . 2_655 ?
N1 C2 N1 47.3(12) 3_665 2_655 ?
C1 O1 Fe1 122.6(3) . . ?
O1 C1 O1 124.8(5) . 6_765 ?

_refine_diff_density_max         0.420
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.077

_shelx_res_file                  
;
TITL DMAFeF_c2_p04_s_ModelR in R-3c
    DMAFeF_c2_p04_s_ModelR.res
    created by SHELXL-2016/6 at 15:24:08 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41111   8.022507   8.022507  21.107594  90.0000  90.0000 120.0000
ZERR    6.00   0.000578   0.000578   0.001614   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 0 2 4
OMIT 0 1 2
ACTA

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.047000    6.996600
FVAR       3.51031
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.03864    0.03864 =
         0.03316    0.00000    0.00000    0.01932
N1    3    0.745197    0.333333    0.083333    10.16667    0.05215    0.04457 =
         0.08231   -0.01040   -0.00520    0.02229
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.780517    0.244914    0.090639    10.33333   -1.20000
C2    1    0.666667    0.333333    0.026264    10.33333    0.09045    0.09045 =
         0.03782    0.00000    0.00000    0.04523
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.543809    0.252038   -0.005536    11.00000   -1.20000
O1    4    0.867135    0.306026    0.277801    11.00000    0.05133    0.04625 =
         0.05222    0.00496    0.01369    0.02530
C1    1    1.000000    0.443712    0.250000    10.50000    0.04274    0.04115 =
         0.04316    0.00084    0.00167    0.02137
AFIX  43
H1    2    1.000001    0.559636    0.250000    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c2_p04_s_ModelR in R-3c
REM R1 =  0.0522 for     214 Fo > 4sig(Fo)  and  0.0648 for all     270 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0470      6.9918

REM Highest difference peak  0.420,  deepest hole -0.423,  1-sigma level  0.077
Q1    1   0.8600  0.5579  0.2784  11.00000  0.05    0.39
Q2    1   0.7523  0.2389  0.3060  11.00000  0.05    0.34
Q3    1   0.7357  0.2534  0.3569  11.00000  0.05    0.32
Q4    1   0.7102  0.1434  0.0565  11.00000  0.05    0.27
Q5    1   1.0482  0.5892  0.2807  11.00000  0.05    0.23
Q6    1   0.9106  0.4547  0.2861  11.00000  0.05    0.22
Q7    1   0.8214  0.2927  0.1287  11.00000  0.05    0.21
Q8    1   0.9619  0.5159  0.2976  11.00000  0.05    0.20
Q9    1   0.7166  0.1662  0.3223  11.00000  0.05    0.20
Q10   1   0.8243  0.1951  0.2577  11.00000  0.05    0.19
Q11   1   0.6667  0.3333 -0.0254  10.33333  0.05    0.19
Q12   1   0.9080  0.2244  0.1357  11.00000  0.05    0.17
Q13   1   0.7172  0.1820  0.0801  11.00000  0.05    0.17
Q14   1   0.6667  0.2738  0.0833  10.50000  0.05    0.17
Q15   1   0.9280  0.3734  0.3053  11.00000  0.05    0.16
Q16   1   0.9416  0.3598  0.3475  11.00000  0.05    0.16
Q17   1   0.8756  0.2448  0.0509  11.00000  0.05    0.16
Q18   1   0.7170  0.1897  0.2339  11.00000  0.05    0.15
Q19   1   0.9272  0.4361  0.3239  11.00000  0.05    0.15
Q20   1   0.7703  0.2911  0.2539  11.00000  0.05    0.15
;
_shelx_res_checksum              31641

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c2_p04       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.731 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c2_p04       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.50 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT088_DMAFeF_c2_p04       
;
PROBLEM: Poor Data / Parameter Ratio ....................       8.71 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. Additionally,
the positioning of the hydrogen atoms for the dynamically disordered 
(CH3)2NH2 unit could not be performed with standard AFIX commands. Instead
distance restraints are used which increases the number of parameters as the
hydrogen positions are refined.
;
_vrf_PLAT415_DMAFeF_c2_p04       
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               2.10 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c2_p04       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 62 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMAFeF_c2_p04       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAFeF_c1_p08
_database_code_depnum_ccdc_archive 'CCDC 1837762'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   7.9495(7)
_cell_length_b                   7.9495(7)
_cell_length_c                   20.5428(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1124.3(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    193
_cell_measurement_theta_min      3.4270
_cell_measurement_theta_max      15.1440

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.449
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83404
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '6.45 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            737
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.964
_diffrn_reflns_theta_max         19.749
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.533
_diffrn_measured_fraction_theta_full 0.823
_diffrn_reflns_Laue_measured_fraction_max 0.533
_diffrn_reflns_Laue_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.533
_diffrn_reflns_point_group_measured_fraction_full 0.823
_reflns_number_total             314
_reflns_number_gt                243
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+3.4165P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         314
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1301
_refine_ls_wR_factor_gt          0.1150
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0391(5) Uani 1 6 d S T P . .
N1 N 0.740(2) 0.333333 0.083333 0.065(4) Uani 0.3333 2 d DS T P . .
H3 H 0.787(11) 0.262(16) 0.101(7) 0.078 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0254(4) 0.087(4) Uani 1 3 d DS T P . .
H2 H 0.571(7) 0.185(4) 0.009(3) 0.105 Uiso 1 1 d D U . . .
O1 O 0.8639(4) 0.2994(4) 0.27726(14) 0.0529(8) Uani 1 1 d . . . . .
C1 C 1.000000 0.4407(7) 0.250000 0.0440(10) Uani 1 2 d S T P . .
H1 H 0.999998 0.557669 0.249998 0.053 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0412(6) 0.0412(6) 0.0347(6) 0.000 0.000 0.0206(3)
N1 0.055(6) 0.056(8) 0.084(11) -0.006(11) -0.003(6) 0.028(4)
C2 0.112(6) 0.112(6) 0.037(4) 0.000 0.000 0.056(3)
O1 0.0533(16) 0.0508(16) 0.0537(14) 0.0040(12) 0.0138(12) 0.0254(13)
C1 0.044(3) 0.047(2) 0.039(2) 0.0005(9) 0.0010(19) 0.0221(13)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.069(3) 31_655 ?
Fe1 O1 2.069(3) . ?
Fe1 O1 2.069(3) 33_545 ?
Fe1 O1 2.069(3) 3_665 ?
Fe1 O1 2.069(3) 32 ?
Fe1 O1 2.069(3) 2_655 ?
N1 N1 1.00(3) 3_665 ?
N1 N1 1.00(3) 2_655 ?
N1 C2 1.323(10) 16_544 ?
N1 C2 1.323(10) . ?
O1 C1 1.237(4) . ?

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 Fe1 O1 180.0 31_655 . ?
O1 Fe1 O1 92.02(12) 31_655 33_545 ?
O1 Fe1 O1 87.98(12) . 33_545 ?
O1 Fe1 O1 87.98(12) 31_655 3_665 ?
O1 Fe1 O1 92.02(12) . 3_665 ?
O1 Fe1 O1 180.0 33_545 3_665 ?
O1 Fe1 O1 92.02(12) 31_655 32 ?
O1 Fe1 O1 87.98(12) . 32 ?
O1 Fe1 O1 92.02(12) 33_545 32 ?
O1 Fe1 O1 87.98(12) 3_665 32 ?
O1 Fe1 O1 87.98(12) 31_655 2_655 ?
O1 Fe1 O1 92.02(12) . 2_655 ?
O1 Fe1 O1 87.98(12) 33_545 2_655 ?
O1 Fe1 O1 92.02(12) 3_665 2_655 ?
O1 Fe1 O1 180.0 32 2_655 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 67.7(5) 3_665 16_544 ?
N1 N1 C2 67.7(5) 2_655 16_544 ?
N1 N1 C2 67.7(5) 3_665 . ?
N1 N1 C2 67.7(5) 2_655 . ?
C2 N1 C2 128.1(13) 16_544 . ?
N1 C2 N1 44.6(11) . 3_665 ?
N1 C2 N1 44.6(11) . 2_655 ?
N1 C2 N1 44.6(11) 3_665 2_655 ?
C1 O1 Fe1 120.6(3) . . ?
O1 C1 O1 123.8(5) 6_765 . ?

_refine_diff_density_max         0.453
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.077

_shelx_res_file                  
;
TITL DMAFeF_c1_p08_s_ModelR in R-3c
    DMAFeF_c1_p08_s_ModelR.res
    created by SHELXL-2016/6 at 17:32:16 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41111   7.949501   7.949501  20.542804  90.0000  90.0000 120.0000
ZERR    6.00   0.000652   0.000652   0.001277   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 0 2 4
OMIT 0 1 2
ACTA

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.053400    3.416500
FVAR       3.74201
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.04123    0.04123 =
         0.03469    0.00000    0.00000    0.02062
N1    3    0.739541    0.333333    0.083333    10.16667    0.05471    0.05568 =
         0.08370   -0.00568   -0.00284    0.02784
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.786744    0.261564    0.100795    10.33333   -1.20000
C2    1    0.666667    0.333333    0.025441    10.33333    0.11227    0.11227 =
         0.03676    0.00000    0.00000    0.05613
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.570985    0.184590    0.008917    11.00000   -1.20000
O1    4    0.863939    0.299357    0.277262    11.00000    0.05326    0.05081 =
         0.05374    0.00395    0.01382    0.02541
C1    1    1.000000    0.440681    0.250000    10.50000    0.04427    0.04735 =
         0.03930    0.00049    0.00098    0.02213
AFIX  43
H1    2    0.999998    0.557669    0.249998    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c1_p08_s_ModelR in R-3c
REM R1 =  0.0475 for     243 Fo > 4sig(Fo)  and  0.0601 for all     314 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0535      3.3848

REM Highest difference peak  0.453,  deepest hole -0.327,  1-sigma level  0.077
Q1    1   0.7386  0.2588  0.3558  11.00000  0.05    0.45
Q2    1   0.8607  0.5607  0.2764  11.00000  0.05    0.31
Q3    1   0.5784  0.1696  0.3473  11.00000  0.05    0.28
Q4    1   0.5000  0.0000  0.0000  10.50000  0.05    0.25
Q5    1   0.6667  0.3333 -0.0099  10.33333  0.05    0.25
Q6    1   0.9517  0.4999  0.2894  11.00000  0.05    0.21
Q7    1   1.0256  0.5733  0.2856  11.00000  0.05    0.20
Q8    1   0.7248  0.1238  0.0755  11.00000  0.05    0.19
Q9    1   0.9724  0.3689  0.3462  11.00000  0.05    0.19
Q10   1   0.7929  0.3743  0.2587  11.00000  0.05    0.17
Q11   1   1.1190  0.6557  0.2701  11.00000  0.05    0.17
Q12   1   1.0362  0.6896  0.2589  11.00000  0.05    0.17
Q13   1   0.4251 -0.0108  0.0186  11.00000  0.05    0.17
Q14   1   0.8571  0.2395  0.2941  11.00000  0.05    0.17
Q15   1   0.8308  0.1916  0.2558  11.00000  0.05    0.15
Q16   1   0.6667  0.3333 -0.0691  10.33333  0.05    0.15
Q17   1   0.8939  0.2384  0.1158  11.00000  0.05    0.15
Q18   1   0.4755  0.2292  0.0304  11.00000  0.05    0.14
Q19   1   0.8802  0.2145  0.3391  11.00000  0.05    0.14
Q20   1   0.9430  0.6785  0.2760  11.00000  0.05    0.14
;
_shelx_res_checksum              61848

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c1_p08       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.823 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c1_p08       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.79 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c1_p08       
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.20 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c1_p08       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 39 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMAFeF_c1_p08       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAMnF_c3_p01_s
_database_code_depnum_ccdc_archive 'CCDC 1837765'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1791 0.2616 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.30764(16)
_cell_length_b                   8.30764(16)
_cell_length_c                   22.6507(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1353.84(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    233
_cell_measurement_theta_min      2.6490
_cell_measurement_theta_max      16.9690

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_F_000             726
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.327
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82836
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '0.58 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            774
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.837
_diffrn_reflns_theta_max         19.696
_diffrn_reflns_theta_full        14.283
_diffrn_measured_fraction_theta_max 0.500
_diffrn_measured_fraction_theta_full 0.834
_diffrn_reflns_Laue_measured_fraction_max 0.500
_diffrn_reflns_Laue_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.500
_diffrn_reflns_point_group_measured_fraction_full 0.834
_reflns_number_total             349
_reflns_number_gt                303
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0312P)²+1.6555P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         349
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mn1 Mn 0.666667 0.333333 0.333333 0.0224(2) Uani 1 6 d S T P . .
N1 N 0.7504(9) 0.333333 0.083333 0.0392(17) Uani 0.3333 2 d DS T P . .
H3 H 0.762(8) 0.233(5) 0.079(4) 0.047 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0298(2) 0.0600(14) Uani 1 3 d DS T P . .
H2 H 0.543(3) 0.199(3) 0.0232(13) 0.072 Uiso 1 1 d D U . . .
O1 O 0.8758(2) 0.3200(2) 0.27873(6) 0.0378(4) Uani 1 1 d . . . . .
C1 C 1.000000 0.4490(3) 0.250000 0.0305(5) Uani 1 2 d S T P . .
H1 H 0.999999 0.560974 0.249999 0.037 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0225(3) 0.0225(3) 0.0221(3) 0.000 0.000 0.01127(14)
N1 0.029(2) 0.022(3) 0.064(4) -0.007(4) -0.004(2) 0.0109(15)
C2 0.069(2) 0.069(2) 0.0422(19) 0.000 0.000 0.0345(11)
O1 0.0350(8) 0.0362(7) 0.0427(7) 0.0077(7) 0.0158(7) 0.0183(6)
C1 0.0300(12) 0.0267(8) 0.0358(11) 0.0007(6) 0.0014(12) 0.0150(6)

_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
Mn1 O1 2.1805(14) 31_655 ?
Mn1 O1 2.1806(14) . ?
Mn1 O1 2.1806(14) 33_545 ?
Mn1 O1 2.1806(14) 3_665 ?
Mn1 O1 2.1806(14) 32 ?
Mn1 O1 2.1806(14) 2_655 ?
N1 N1 1.205(14) 3_665 ?
N1 N1 1.205(14) 2_655 ?
N1 C2 1.398(6) 16_544 ?
N1 C2 1.398(6) . ?
O1 C1 1.2374(19) . ?

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 Mn1 O1 180.00(6) 31_655 . ?
O1 Mn1 O1 91.00(5) 31_655 33_545 ?
O1 Mn1 O1 89.00(5) . 33_545 ?
O1 Mn1 O1 89.00(5) 31_655 3_665 ?
O1 Mn1 O1 91.00(5) . 3_665 ?
O1 Mn1 O1 180.0 33_545 3_665 ?
O1 Mn1 O1 91.00(5) 31_655 32 ?
O1 Mn1 O1 89.00(5) . 32 ?
O1 Mn1 O1 91.00(5) 33_545 32 ?
O1 Mn1 O1 89.00(5) 3_665 32 ?
O1 Mn1 O1 89.00(5) 31_655 2_655 ?
O1 Mn1 O1 91.00(5) . 2_655 ?
O1 Mn1 O1 89.00(5) 33_545 2_655 ?
O1 Mn1 O1 91.00(5) 3_665 2_655 ?
O1 Mn1 O1 180.0 32 2_655 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 64.5(3) 3_665 16_544 ?
N1 N1 C2 64.5(3) 2_655 16_544 ?
N1 N1 C2 64.5(3) 3_665 . ?
N1 N1 C2 64.5(3) 2_655 . ?
C2 N1 C2 120.3(6) 16_544 . ?
N1 C2 N1 51.1(5) . 3_665 ?
N1 C2 N1 51.1(5) . 2_655 ?
N1 C2 N1 51.1(5) 3_665 2_655 ?
C1 O1 Mn1 126.47(15) . . ?
O1 C1 O1 126.5(3) 6_765 . ?

_refine_diff_density_max         0.228
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.058

_shelx_res_file                  
;
TITL DMAMnF_c3_p01_s in R-3c
    DMAMnF_c3_p01_s.res
    created by SHELXL-2016/6 at 10:13:38 on 23-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41119   8.307645   8.307645  22.650654  90.0000  90.0000 120.0000
ZERR    6.00   0.000162   0.000162   0.000261   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Mn
DISP $C -0.00006  0.00048  5.14212!source kissel
DISP $H -0.00003  0.00000  0.64130!source kissel
DISP $N  0.00062  0.00099  7.19266!source kissel
DISP $O  0.00180  0.00183 10.15895!source kissel
DISP $Mn  0.17908  0.26161 636.31605!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
TEMP 20
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.031200    1.655500
FVAR       2.94038
MOLE   1
MN1   5    0.666667    0.333333    0.333333    10.16667    0.02254    0.02254 =
         0.02209    0.00000    0.00000    0.01127
N1    3    0.750411    0.333333    0.083333    10.16667    0.02933    0.02172 =
         0.06405   -0.00748   -0.00374    0.01086
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.762386    0.233031    0.078928    10.33333   -1.20000
C2    1    0.666667    0.333333    0.029815    10.33333    0.06891    0.06891 =
         0.04220    0.00000    0.00000    0.03446
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.542550    0.199483    0.023200    11.00000   -1.20000
O1    4    0.875845    0.319955    0.278734    11.00000    0.03504    0.03618 =
         0.04274    0.00773    0.01583    0.01833
C1    1    1.000000    0.449029    0.250000    10.50000    0.02999    0.02673 =
         0.03583    0.00069    0.00137    0.01500
AFIX  43
H1    2    0.999999    0.560974    0.249999    10.50000   -1.20000
AFIX   0
HKLF 4




REM  DMAMnF_c3_p01_s in R-3c
REM R1 =  0.0281 for     303 Fo > 4sig(Fo)  and  0.0331 for all     349 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0314      1.6376

REM Highest difference peak  0.228,  deepest hole -0.274,  1-sigma level  0.058
Q1    1   0.9707  0.3963  0.2978  11.00000  0.05    0.23
Q2    1   0.5000  0.0000  0.0000  10.50000  0.05    0.20
Q3    1   0.6179  0.2684 -0.0082  11.00000  0.05    0.20
Q4    1   1.0497  0.6353  0.2815  11.00000  0.05    0.19
Q5    1   0.9043  0.2514  0.2965  11.00000  0.05    0.17
Q6    1   0.9775  0.6451  0.2841  11.00000  0.05    0.17
Q7    1   0.8701  0.5637  0.2816  11.00000  0.05    0.17
Q8    1   1.1093  0.5859  0.2680  11.00000  0.05    0.16
Q9    1   0.7825  0.3338  0.2937  11.00000  0.05    0.16
Q10   1   0.8700  0.5573  0.3068  11.00000  0.05    0.15
Q11   1   0.8306  0.3443  0.2680  11.00000  0.05    0.15
Q12   1   0.6667  0.2273  0.0833  10.50000  0.05    0.15
Q13   1   0.7880  0.2295  0.3306  11.00000  0.05    0.14
Q14   1   0.8684  0.2610  0.0459  11.00000  0.05    0.14
Q15   1   0.5063  0.0987  0.0459  11.00000  0.05    0.13
Q16   1   0.5390  0.2083  0.3585  11.00000  0.05    0.12
Q17   1   0.7407  0.2270  0.0413  11.00000  0.05    0.11
Q18   1   0.9000  0.2203  0.2748  11.00000  0.05    0.11
Q19   1   0.4259  0.0325  0.0049  11.00000  0.05    0.10
Q20   1   0.9053  0.2545  0.3323  11.00000  0.05    0.10
;
_shelx_res_checksum              53887

# start Validation Reply Form
_vrf_PLAT029_DMAMnF_c3_p01_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.834 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAMnF_c3_p01_s     
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.86 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAMnF_c3_p01_s     
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.50 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances.  In addition, as the (CH3)2NH2 unit
is dynamically disordered, accurate positioning of the H atoms may not
always be possible.
;
_vrf_PLAT911_DMAMnF_c3_p01_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 44 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT303_DMAMnF_c3_p01_s     
;
PROBLEM: Full Occupancy Atom H2        with # Connections       1.33 Check 
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT978_DMAMnF_c3_p01_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAFeF_c2_p01
_database_code_depnum_ccdc_archive 'CCDC 1837755'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.17987(18)
_cell_length_b                   8.17987(18)
_cell_length_c                   22.0315(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1276.63(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    296
_cell_measurement_theta_min      2.8820
_cell_measurement_theta_max      17.0800

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.395
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79703
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '1.11 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            812
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.881
_diffrn_reflns_theta_max         20.414
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.398
_diffrn_measured_fraction_theta_full 0.737
_diffrn_reflns_Laue_measured_fraction_max 0.398
_diffrn_reflns_Laue_measured_fraction_full 0.737
_diffrn_reflns_point_group_measured_fraction_max 0.398
_diffrn_reflns_point_group_measured_fraction_full 0.737
_reflns_number_total             293
_reflns_number_gt                259
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²+4.0368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         293
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0894
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.194
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0235(3) Uani 1 6 d S T P . .
N1 N 0.7518(15) 0.333333 0.083333 0.043(3) Uani 0.3333 2 d DS T P . .
H3 H 0.767(9) 0.232(6) 0.085(6) 0.052 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0277(4) 0.065(2) Uani 1 3 d DS T P . .
H2 H 0.566(5) 0.193(3) 0.010(2) 0.078 Uiso 1 1 d D U . . .
O1 O 0.8723(3) 0.3183(3) 0.27870(10) 0.0378(5) Uani 1 1 d . . . . .
C1 C 1.000000 0.4523(5) 0.250000 0.0320(8) Uani 1 2 d S T P . .
H1 H 0.999998 0.565995 0.249999 0.038 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0211(4) 0.0211(4) 0.0283(5) 0.000 0.000 0.01054(19)
N1 0.036(4) 0.023(5) 0.066(8) -0.004(5) -0.002(3) 0.011(3)
C2 0.073(3) 0.073(3) 0.048(4) 0.000 0.000 0.0367(17)
O1 0.0340(11) 0.0321(11) 0.0462(12) 0.0047(8) 0.0119(8) 0.0157(9)
C1 0.0244(18) 0.0273(14) 0.043(2) 0.0010(7) 0.0021(14) 0.0122(9)

_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
Fe1 O1 2.1215(19) 31_655 ?
Fe1 O1 2.1216(19) 33_545 ?
Fe1 O1 2.1216(19) . ?
Fe1 O1 2.1216(19) 3_665 ?
Fe1 O1 2.1216(19) 32 ?
Fe1 O1 2.1216(19) 2_655 ?
N1 N1 1.21(2) 3_665 ?
N1 N1 1.21(2) 2_655 ?
N1 C2 1.409(10) 16_544 ?
N1 C2 1.409(10) . ?
O1 C1 1.244(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 Fe1 O1 90.98(9) 31_655 33_545 ?
O1 Fe1 O1 180.00(10) 31_655 . ?
O1 Fe1 O1 89.02(9) 33_545 . ?
O1 Fe1 O1 89.02(9) 31_655 3_665 ?
O1 Fe1 O1 180.0 33_545 3_665 ?
O1 Fe1 O1 90.98(9) . 3_665 ?
O1 Fe1 O1 90.98(9) 31_655 32 ?
O1 Fe1 O1 90.98(9) 33_545 32 ?
O1 Fe1 O1 89.02(8) . 32 ?
O1 Fe1 O1 89.02(9) 3_665 32 ?
O1 Fe1 O1 89.02(9) 31_655 2_655 ?
O1 Fe1 O1 89.02(9) 33_545 2_655 ?
O1 Fe1 O1 90.98(9) . 2_655 ?
O1 Fe1 O1 90.98(8) 3_665 2_655 ?
O1 Fe1 O1 180.0 32 2_655 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 64.6(4) 3_665 16_544 ?
N1 N1 C2 64.6(4) 2_655 16_544 ?
N1 N1 C2 64.7(4) 3_665 . ?
N1 N1 C2 64.7(4) 2_655 . ?
C2 N1 C2 120.7(9) 16_544 . ?
N1 C2 N1 50.7(8) . 3_665 ?
N1 C2 N1 50.7(8) . 2_655 ?
N1 C2 N1 50.7(8) 3_665 2_655 ?
C1 O1 Fe1 125.31(19) . . ?
O1 C1 O1 125.0(4) . 6_765 ?

_refine_diff_density_max         0.285
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.068

_shelx_res_file                  
;
TITL DMAFeF_c2_p01_s2_ModelR in R-3c
    DMAFeF_c2_p01_s2_ModelR.res
    created by SHELXL-2016/6 at 14:49:01 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41111   8.179871   8.179871  22.031466  90.0000  90.0000 120.0000
ZERR    6.00   0.000179   0.000179   0.000606   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 0 2 4
OMIT 0 1 2
ACTA

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.033400    4.036800
FVAR       3.31104
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.02108    0.02108 =
         0.02835    0.00000    0.00000    0.01054
N1    3    0.751841    0.333333    0.083333    10.16667    0.03572    0.02288 =
         0.06649   -0.00385   -0.00192    0.01144
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.767150    0.232215    0.084826    10.33333   -1.20000
C2    1    0.666667    0.333333    0.027733    10.33333    0.07349    0.07349 =
         0.04809    0.00000    0.00000    0.03675
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.566182    0.193446    0.010322    11.00000   -1.20000
O1    4    0.872334    0.318309    0.278695    11.00000    0.03405    0.03208 =
         0.04623    0.00473    0.01193    0.01573
C1    1    1.000000    0.452302    0.250000    10.50000    0.02437    0.02728 =
         0.04323    0.00105    0.00209    0.01219
AFIX  43
H1    2    0.999998    0.565995    0.249999    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c2_p01_s2_ModelR in R-3c
REM R1 =  0.0351 for     259 Fo > 4sig(Fo)  and  0.0405 for all     293 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0333      4.0431

REM Highest difference peak  0.285,  deepest hole -0.445,  1-sigma level  0.068
Q1    1   1.0490  0.5747  0.2852  11.00000  0.05    0.29
Q2    1   1.0365  0.6131  0.2739  11.00000  0.05    0.24
Q3    1   0.7414  0.2428  0.3027  11.00000  0.05    0.23
Q4    1   0.8701  0.5667  0.2814  11.00000  0.05    0.22
Q5    1   0.9182  0.3704  0.2982  11.00000  0.05    0.20
Q6    1   0.8085  0.3556  0.3157  11.00000  0.05    0.20
Q7    1   0.7163  0.2841  0.2849  11.00000  0.05    0.19
Q8    1   0.4372 -0.0014  0.0045  11.00000  0.05    0.18
Q9    1   0.4877  0.2081  0.0320  11.00000  0.05    0.18
Q10   1   1.1437  0.5564  0.2603  11.00000  0.05    0.17
Q11   1   0.9242  0.4074  0.2783  11.00000  0.05    0.16
Q12   1   0.9958  0.3366  0.3153  11.00000  0.05    0.16
Q13   1   0.8560  0.2445  0.3336  11.00000  0.05    0.15
Q14   1   0.8017  0.1407  0.0908  11.00000  0.05    0.15
Q15   1   0.4006  0.1865 -0.0120  11.00000  0.05    0.14
Q16   1   0.7174  0.1615  0.0669  11.00000  0.05    0.14
Q17   1   0.6850  0.2511 -0.0551  11.00000  0.05    0.14
Q18   1   0.6667  0.3333  0.4127  10.33333  0.05    0.13
Q19   1   1.0000  0.6623  0.2500  10.50000  0.05    0.13
Q20   1   0.9126  0.2453  0.1191  11.00000  0.05    0.13
;
_shelx_res_checksum              46103

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c2_p01       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.737 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c2_p01       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.78 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c2_p01       
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.66 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c2_p01       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 67 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT088_DMAFeF_c2_p01       
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.45 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. Additionally,
the positioning of the hydrogen atoms for the dynamically disordered 
(CH3)2NH2 unit could not be performed with standard AFIX commands. Instead
distance restraints are used which increases the number of parameters as the
hydrogen positions are refined.
;
_vrf_PLAT913_DMAFeF_c2_p01       
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....          4 Note  
RESPONSE: The overflow reflections were omitted from the refinement.
;
_vrf_PLAT978_DMAFeF_c2_p01       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMAFeF_c1_p07
_database_code_depnum_ccdc_archive 'CCDC 1837761'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   7.9763(6)
_cell_length_b                   7.9763(6)
_cell_length_c                   20.6525(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1137.91(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    224
_cell_measurement_theta_min      2.0540
_cell_measurement_theta_max      16.2590

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.443
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80701
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '6.02 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            749
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.954
_diffrn_reflns_theta_max         19.649
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.541
_diffrn_measured_fraction_theta_full 0.828
_diffrn_reflns_Laue_measured_fraction_max 0.541
_diffrn_reflns_Laue_measured_fraction_full 0.828
_diffrn_reflns_point_group_measured_fraction_max 0.541
_diffrn_reflns_point_group_measured_fraction_full 0.828
_reflns_number_total             318
_reflns_number_gt                253
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0467P)²+3.5141P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         318
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1098
_refine_ls_wR_factor_gt          0.0998
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0329(4) Uani 1 6 d S T P . .
N1 N 0.7404(17) 0.333333 0.083333 0.060(3) Uani 0.3333 2 d DS T P . .
H3 H 0.776(9) 0.243(7) 0.084(8) 0.072 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0254(3) 0.076(3) Uani 1 3 d DS T P . .
H2 H 0.564(6) 0.183(3) 0.013(3) 0.092 Uiso 1 1 d D U . . .
O1 O 0.8642(3) 0.2999(3) 0.27740(11) 0.0460(6) Uani 1 1 d . . . . .
C1 C 1.000000 0.4401(6) 0.250000 0.0384(9) Uani 1 2 d S T P . .
H1 H 1.000004 0.556688 0.250002 0.046 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0342(5) 0.0342(5) 0.0302(5) 0.000 0.000 0.0171(2)
N1 0.049(5) 0.046(6) 0.084(9) -0.006(10) -0.003(5) 0.023(3)
C2 0.098(4) 0.098(4) 0.033(3) 0.000 0.000 0.049(2)
O1 0.0459(13) 0.0438(13) 0.0477(12) 0.0048(9) 0.0126(10) 0.0220(10)
C1 0.039(2) 0.0387(16) 0.0373(18) 0.0005(8) 0.0011(15) 0.0197(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
Fe1 O1 2.076(2) 3_665 ?
Fe1 O1 2.076(2) 2_655 ?
Fe1 O1 2.076(2) . ?
Fe1 O1 2.076(2) 31_655 ?
Fe1 O1 2.076(2) 33_545 ?
Fe1 O1 2.076(2) 32 ?
N1 N1 1.02(2) 3_665 ?
N1 N1 1.02(2) 2_655 ?
N1 C2 1.334(9) 16_544 ?
N1 C2 1.334(9) . ?
O1 C1 1.238(3) . ?

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 Fe1 O1 92.04(10) 3_665 2_655 ?
O1 Fe1 O1 92.04(10) 3_665 . ?
O1 Fe1 O1 92.04(10) 2_655 . ?
O1 Fe1 O1 87.96(10) 3_665 31_655 ?
O1 Fe1 O1 87.96(10) 2_655 31_655 ?
O1 Fe1 O1 180.0 . 31_655 ?
O1 Fe1 O1 180.0 3_665 33_545 ?
O1 Fe1 O1 87.97(10) 2_655 33_545 ?
O1 Fe1 O1 87.97(10) . 33_545 ?
O1 Fe1 O1 92.03(10) 31_655 33_545 ?
O1 Fe1 O1 87.96(10) 3_665 32 ?
O1 Fe1 O1 180.0 2_655 32 ?
O1 Fe1 O1 87.97(10) . 32 ?
O1 Fe1 O1 92.03(10) 31_655 32 ?
O1 Fe1 O1 92.03(10) 33_545 32 ?
N1 N1 N1 60.0 3_665 2_655 ?
N1 N1 C2 67.5(5) 3_665 16_544 ?
N1 N1 C2 67.5(5) 2_655 16_544 ?
N1 N1 C2 67.5(5) 3_665 . ?
N1 N1 C2 67.5(5) 2_655 . ?
C2 N1 C2 127.7(11) 16_544 . ?
N1 C2 N1 44.9(9) . 3_665 ?
N1 C2 N1 44.9(9) . 2_655 ?
N1 C2 N1 44.9(9) 3_665 2_655 ?
C1 O1 Fe1 121.1(2) . . ?
O1 C1 O1 124.5(4) . 6_765 ?

_refine_diff_density_max         0.401
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.075

_shelx_res_file                  
;
TITL DMAFeF_c1_p07_s_ModelR in R-3c
    DMAFeF_c1_p07_s_ModelR.res
    created by SHELXL-2016/6 at 17:23:10 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41111   7.976324   7.976324  20.652535  90.0000  90.0000 120.0000
ZERR    6.00   0.000557   0.000557   0.001223   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 0 2 4
OMIT 0 1 2
ACTA

LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.046700    3.514100
FVAR       3.75814
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.03423    0.03423 =
         0.03021    0.00000    0.00000    0.01711
N1    3    0.740414    0.333333    0.083333    10.16667    0.04896    0.04584 =
         0.08385   -0.00635   -0.00318    0.02292
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.776205    0.242906    0.083528    10.33333   -1.20000
C2    1    0.666667    0.333333    0.025370    10.33333    0.09787    0.09787 =
         0.03308    0.00000    0.00000    0.04894
DFIX 1.1 0.01 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.564250    0.183201    0.013071    11.00000   -1.20000
O1    4    0.864241    0.299912    0.277401    11.00000    0.04590    0.04375 =
         0.04766    0.00475    0.01264    0.02195
C1    1    1.000000    0.440091    0.250000    10.50000    0.03946    0.03870 =
         0.03731    0.00053    0.00106    0.01973
AFIX  43
H1    2    1.000004    0.556688    0.250002    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c1_p07_s_ModelR in R-3c
REM R1 =  0.0421 for     253 Fo > 4sig(Fo)  and  0.0510 for all     318 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0467      3.5244

REM Highest difference peak  0.401,  deepest hole -0.290,  1-sigma level  0.075
Q1    1   0.7517  0.4875  0.3533  11.00000  0.05    0.40
Q2    1   0.6667  0.3333 -0.0222  10.33333  0.05    0.37
Q3    1   0.8804  0.5829  0.2794  11.00000  0.05    0.33
Q4    1   0.7494  0.2532  0.3156  11.00000  0.05    0.31
Q5    1   0.5000  0.0000  0.0000  10.50000  0.05    0.29
Q6    1   0.6667  0.3333  0.3887  10.33333  0.05    0.20
Q7    1   0.8620  0.2535  0.2879  11.00000  0.05    0.19
Q8    1   0.6667  0.2689  0.0833  10.50000  0.05    0.18
Q9    1   0.8969  0.3633  0.2546  11.00000  0.05    0.18
Q10   1   1.0669  0.6191  0.2824  11.00000  0.05    0.17
Q11   1   0.5849  0.0318 -0.0198  11.00000  0.05    0.17
Q12   1   1.0049  0.3251  0.2952  11.00000  0.05    0.16
Q13   1   0.8966  0.3481  0.3009  11.00000  0.05    0.16
Q14   1   0.6667  0.3333 -0.0679  10.33333  0.05    0.15
Q15   1   0.9379  0.6345  0.3154  11.00000  0.05    0.15
Q16   1   0.9454  0.6388  0.2765  11.00000  0.05    0.15
Q17   1   0.5723  0.2896  0.0006  11.00000  0.05    0.15
Q18   1   0.5903  0.3292  0.3787  11.00000  0.05    0.15
Q19   1   0.8961  0.2089  0.2750  11.00000  0.05    0.15
Q20   1   0.4705  0.2241  0.0257  11.00000  0.05    0.15
;
_shelx_res_checksum              20149

# start Validation Reply Form
_vrf_PLAT029_DMAFeF_c1_p07       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.828 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT413_DMAFeF_c1_p07       
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.84 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c1_p07       
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.76 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT911_DMAFeF_c1_p07       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 38 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMAFeF_c1_p07       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMACuF_c1_p03
_database_code_depnum_ccdc_archive 'CCDC 1837738'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c1_p03       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.599 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMACuF_c1_p03       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        305 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMACuF_c1_p03       
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.3229(5)
_cell_length_b                   8.5761(8)
_cell_length_c                   8.6487(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.432(5)
_cell_angle_gamma                90
_cell_volume                     836.07(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    248
_cell_measurement_theta_min      1.7270
_cell_measurement_theta_max      17.2010

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.588
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         '1.14 GPa'
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1251
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.726
_diffrn_reflns_theta_max         20.522
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.344
_diffrn_measured_fraction_theta_full 0.599
_diffrn_reflns_Laue_measured_fraction_max 0.344
_diffrn_reflns_Laue_measured_fraction_full 0.599
_diffrn_reflns_point_group_measured_fraction_max 0.344
_diffrn_reflns_point_group_measured_fraction_full 0.599
_reflns_number_total             752
_reflns_number_gt                551
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+1.4627P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         752
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0229(2) Uani 1 2 d S . P . .
O2 O 0.34783(18) 0.6090(3) 0.5070(3) 0.0295(6) Uani 1 1 d . . . . .
O1 O 0.4256(2) 0.2274(4) 0.1198(4) 0.0347(7) Uani 1 1 d . . . . .
O3 O 0.4380(2) 0.4124(4) 0.2973(4) 0.0334(7) Uani 1 1 d . . . . .
N1 N 0.250000 0.4383(7) 0.000000 0.0340(11) Uani 1 2 d DS T P . .
H3 H 0.193(4) 0.384(6) -0.044(6) 0.041 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5404(7) 0.500000 0.0243(10) Uani 1 2 d S T P . .
H2 H 0.249999 0.432009 0.499999 0.029 Uiso 1 2 calc R U P . .
C1 C 0.4697(3) 0.2854(5) 0.2433(5) 0.0291(8) Uani 1 1 d . . . . .
H1 H 0.530412 0.230816 0.299625 0.035 Uiso 1 1 calc R U . . .
C3 C 0.1900(4) 0.5312(6) 0.1098(7) 0.0473(12) Uani 1 1 d . . . . .
H4 H 0.152454 0.463250 0.178539 0.057 Uiso 1 1 calc R U . . .
H5 H 0.246877 0.595748 0.169059 0.057 Uiso 1 1 calc R U . . .
H6 H 0.131173 0.595748 0.054148 0.057 Uiso 1 1 calc R U . . .

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
Cu1 0.0152(2) 0.0300(5) 0.0227(5) -0.00249(19) -0.0019(2) 0.00161(19)
O2 0.0179(8) 0.031(2) 0.039(2) -0.0013(10) -0.0005(10) -0.0001(9)
O1 0.0318(11) 0.039(2) 0.032(2) -0.0080(11) -0.0028(12) 0.0033(12)
O3 0.0303(10) 0.041(2) 0.027(2) -0.0059(10) -0.0057(11) 0.0078(11)
N1 0.0290(17) 0.029(4) 0.041(4) 0.000 -0.012(2) 0.000
C2 0.0153(14) 0.029(3) 0.029(3) 0.000 0.0019(18) 0.000
C1 0.0232(12) 0.033(3) 0.030(3) -0.0005(13) -0.0022(14) 0.0007(14)
C3 0.044(2) 0.059(4) 0.040(4) 0.005(2) 0.009(2) 0.001(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
Cu1 O2 1.966(2) . ?
Cu1 O2 1.966(2) 5_666 ?
Cu1 O3 1.974(3) 5_666 ?
Cu1 O3 1.974(3) . ?
Cu1 O1 2.398(3) 4 ?
Cu1 O1 2.398(3) 8 ?
O2 C2 1.250(3) . ?
O1 C1 1.240(5) . ?
O3 C1 1.251(5) . ?
N1 C3 1.456(6) . ?
N1 C3 1.456(6) 2 ?
N1 H3 0.86(4) . ?
N1 H3 0.86(4) 2 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.00(14) . 5_666 ?
O2 Cu1 O3 91.76(11) . 5_666 ?
O2 Cu1 O3 88.24(11) 5_666 5_666 ?
O2 Cu1 O3 88.24(11) . . ?
O2 Cu1 O3 91.76(11) 5_666 . ?
O3 Cu1 O3 180.0 5_666 . ?
O2 Cu1 O1 88.36(11) . 4 ?
O2 Cu1 O1 91.64(11) 5_666 4 ?
O3 Cu1 O1 87.96(12) 5_666 4 ?
O3 Cu1 O1 92.04(12) . 4 ?
O2 Cu1 O1 91.64(11) . 8 ?
O2 Cu1 O1 88.36(11) 5_666 8 ?
O3 Cu1 O1 92.04(12) 5_666 8 ?
O3 Cu1 O1 87.96(12) . 8 ?
O1 Cu1 O1 180.0 4 8 ?
C2 O2 Cu1 123.4(3) . . ?
C1 O1 Cu1 124.7(2) . 4_545 ?
C1 O3 Cu1 124.9(3) . . ?
C3 N1 C3 113.6(6) . 2 ?
C3 N1 H3 103(4) . . ?
C3 N1 H3 113(4) 2 . ?
C3 N1 H3 113(4) . 2 ?
C3 N1 H3 103(4) 2 2 ?
H3 N1 H3 114(7) . 2 ?
O2 C2 O2 123.9(5) 2_556 . ?
O2 C2 H2 118.0 2_556 . ?
O2 C2 H2 118.0 . . ?
O1 C1 O3 124.3(4) . . ?
O1 C1 H1 117.8 . . ?
O3 C1 H1 117.8 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.356
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.080

_shelx_res_file                  
;
TITL DMACuF_c1_p03_s_set2 in I2/a
    DMACuF_c1_p03_s_set2.res
    created by SHELXL-2016/6 at 12:15:40 on 27-Sep-2017
REM I2/a (#15 in standard setting)
CELL 0.41108  11.322939   8.576093   8.648704  90.0000  95.4316  90.0000
ZERR    4.00   0.000461   0.000822   0.000772   0.0000   0.0054   0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00
OMIT 0 1 1
SIZE 0.06 0.04 0.03
L.S. 10
ACTA
BOND $H
LIST 4
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.027100    1.462700
FVAR       2.85964
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01521    0.03002 =
         0.02266   -0.00249   -0.00189    0.00161
O2    4    0.347827    0.608983    0.506983    11.00000    0.01791    0.03112 =
         0.03889   -0.00130   -0.00048   -0.00007

O1    4    0.425588    0.227412    0.119805    11.00000    0.03180    0.03936 =
         0.03192   -0.00796   -0.00275    0.00335
O3    4    0.438023    0.412412    0.297270    11.00000    0.03030    0.04107 =
         0.02713   -0.00593   -0.00566    0.00779
N1    3    0.250000    0.438260    0.000000    10.50000    0.02899    0.02936 =
         0.04051    0.00000   -0.01238    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.193307    0.383557   -0.044479    11.00000   -1.20000
C2    1    0.250000    0.540450    0.500000    10.50000    0.01528    0.02898 =
         0.02875    0.00000    0.00193    0.00000
AFIX  43
H2    2    0.249999    0.432009    0.499999    10.50000   -1.20000
AFIX   0
C1    1    0.469722    0.285382    0.243336    11.00000    0.02321    0.03290 =
         0.03043   -0.00049   -0.00221    0.00065
AFIX  43
H1    2    0.530412    0.230816    0.299625    11.00000   -1.20000
AFIX   0
C3    1    0.190018    0.531163    0.109786    11.00000    0.04404    0.05909 =
         0.03966    0.00468    0.00858    0.00119
AFIX  33
H4    2    0.152454    0.463250    0.178539    11.00000   -1.20000
H5    2    0.246877    0.595748    0.169059    11.00000   -1.20000
H6    2    0.131173    0.595748    0.054148    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_p03_s_set2 in I2/a
REM R1 =  0.0337 for     551 Fo > 4sig(Fo)  and  0.0498 for all     752 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0271      1.4667

REM Highest difference peak  0.356,  deepest hole -0.371,  1-sigma level  0.080
Q1    1   0.5097  0.5838  0.5848  11.00000  0.05    0.36
Q2    1   0.4365  0.5827  0.2961  11.00000  0.05    0.33
Q3    1   0.4993  0.5666  0.4239  11.00000  0.05    0.30
Q4    1   0.1537  0.3865  0.5005  11.00000  0.05    0.28
Q5    1   0.4689  0.4748  0.3422  11.00000  0.05    0.28
Q6    1   0.1765  0.3647  0.3022  11.00000  0.05    0.27
Q7    1   0.4342  0.2339  0.0796  11.00000  0.05    0.26
Q8    1   0.3330  0.4114  0.3592  11.00000  0.05    0.24
Q9    1   0.5670  0.4987  0.5471  11.00000  0.05    0.24
Q10   1   0.5064  0.3695  0.3520  11.00000  0.05    0.24
Q11   1   0.3513  0.1665  0.0574  11.00000  0.05    0.24
Q12   1   0.5741  0.2713  0.3902  11.00000  0.05    0.23
Q13   1   0.3827  0.2246  0.1593  11.00000  0.05    0.23
Q14   1   0.1709  0.4385  0.2761  11.00000  0.05    0.22
Q15   1   0.4701  0.6442  0.4776  11.00000  0.05    0.22
Q16   1   0.3953  0.4456  0.3552  11.00000  0.05    0.22
Q17   1   0.2176  0.3415  0.4856  11.00000  0.05    0.22
Q18   1   0.2990  0.4835  0.2553  11.00000  0.05    0.22
Q19   1   0.5088  0.6373  0.5074  11.00000  0.05    0.22
Q20   1   0.0892  0.4850  0.1301  11.00000  0.05    0.21
;
_shelx_res_checksum              64710
####################################################################### 
# 
# 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_DMACuF_c1_p06_s
_database_code_depnum_ccdc_archive 'CCDC 1837741'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_DMACuF_c1_p06_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        286 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMACuF_c1_p06_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info
RESPONSE: There are no C-C bonds in the structure.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4684 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   11.16852(13)
_cell_length_b                   8.4704(3)
_cell_length_c                   8.3956(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.7845(18)
_cell_angle_gamma                90
_cell_volume                     791.46(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    233
_cell_measurement_theta_min      1.9760
_cell_measurement_theta_max      17.4330

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_F_000             500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.621
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         '3.11 GPa'
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            1186
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.747
_diffrn_reflns_theta_max         20.909
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.328
_diffrn_measured_fraction_theta_full 0.601
_diffrn_reflns_Laue_measured_fraction_max 0.328
_diffrn_reflns_Laue_measured_fraction_full 0.601
_diffrn_reflns_point_group_measured_fraction_max 0.328
_diffrn_reflns_point_group_measured_fraction_full 0.601
_reflns_number_total             713
_reflns_number_gt                520
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+3.9178P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         713
_refine_ls_number_parameters     65
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1220
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0277(3) Uani 1 2 d S . P . .
O2 O 0.3488(2) 0.6152(4) 0.5079(5) 0.0349(8) Uani 1 1 d . . . . .
O1 O 0.4222(3) 0.2223(5) 0.1147(5) 0.0389(9) Uani 1 1 d . . . . .
O3 O 0.4369(3) 0.4147(5) 0.2911(5) 0.0374(9) Uani 1 1 d . . . . .
N1 N 0.250000 0.4412(9) 0.000000 0.0423(16) Uani 1 2 d DS T P . .
H3 H 0.183(5) 0.388(8) -0.040(8) 0.051 Uiso 1 1 d D U . . .
C2 C 0.250000 0.5461(9) 0.500000 0.0288(13) Uani 1 2 d S T P . .
H2 H 0.250001 0.436303 0.500003 0.035 Uiso 1 2 calc R U P . .
C1 C 0.4665(4) 0.2837(7) 0.2405(7) 0.0342(11) Uani 1 1 d . . . . .
H1 H 0.525866 0.227842 0.300914 0.041 Uiso 1 1 calc R U . . .
C3 C 0.1877(6) 0.5345(8) 0.1102(9) 0.0528(16) Uani 1 1 d . . . . .
H4 H 0.148126 0.465976 0.180260 0.063 Uiso 1 1 calc R U . . .
H5 H 0.244288 0.599923 0.172143 0.063 Uiso 1 1 calc R U . . .
H6 H 0.129165 0.599925 0.051778 0.063 Uiso 1 1 calc R U . . .

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
Cu1 0.0194(3) 0.0400(7) 0.0231(6) -0.0017(3) -0.0012(3) 0.0011(3)
O2 0.0212(11) 0.045(3) 0.038(3) -0.0016(13) 0.0000(14) 0.0009(13)
O1 0.0356(16) 0.047(3) 0.033(3) -0.0080(14) -0.0037(16) 0.0054(15)
O3 0.0346(15) 0.050(3) 0.027(3) -0.0069(14) -0.0051(16) 0.0056(15)
N1 0.033(2) 0.049(5) 0.043(5) 0.000 -0.007(3) 0.000
C2 0.0194(19) 0.037(4) 0.030(5) 0.000 0.002(2) 0.000
C1 0.0275(17) 0.045(4) 0.029(4) 0.0023(18) -0.0048(19) 0.0002(19)
C3 0.046(3) 0.070(5) 0.044(5) 0.007(3) 0.016(3) 0.001(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
Cu1 O2 1.957(3) 5_666 ?
Cu1 O2 1.957(3) . ?
Cu1 O3 1.972(3) . ?
Cu1 O3 1.972(3) 5_666 ?
Cu1 O1 2.316(4) 4 ?
Cu1 O1 2.316(4) 8 ?
O2 C2 1.246(5) . ?
O1 C1 1.242(6) . ?
O3 C1 1.243(7) . ?
N1 C3 1.440(8) . ?
N1 C3 1.440(8) 2 ?
N1 H3 0.92(5) . ?
N1 H3 0.92(5) 2 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C3 H4 0.9600 . ?
C3 H5 0.9600 . ?
C3 H6 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 5_666 . ?
O2 Cu1 O3 91.86(15) 5_666 . ?
O2 Cu1 O3 88.14(15) . . ?
O2 Cu1 O3 88.14(15) 5_666 5_666 ?
O2 Cu1 O3 91.86(15) . 5_666 ?
O3 Cu1 O3 180.0 . 5_666 ?
O2 Cu1 O1 92.10(14) 5_666 4 ?
O2 Cu1 O1 87.90(14) . 4 ?
O3 Cu1 O1 92.68(16) . 4 ?
O3 Cu1 O1 87.32(16) 5_666 4 ?
O2 Cu1 O1 87.90(14) 5_666 8 ?
O2 Cu1 O1 92.10(14) . 8 ?
O3 Cu1 O1 87.32(16) . 8 ?
O3 Cu1 O1 92.68(16) 5_666 8 ?
O1 Cu1 O1 180.0 4 8 ?
C2 O2 Cu1 121.8(4) . . ?
C1 O1 Cu1 123.9(3) . 4_545 ?
C1 O3 Cu1 123.1(3) . . ?
C3 N1 C3 113.4(8) . 2 ?
C3 N1 H3 95(4) . . ?
C3 N1 H3 117(5) 2 . ?
C3 N1 H3 117(5) . 2 ?
C3 N1 H3 95(4) 2 2 ?
H3 N1 H3 121(9) . 2 ?
O2 C2 O2 123.9(7) 2_556 . ?
O2 C2 H2 118.0 2_556 . ?
O2 C2 H2 118.0 . . ?
O1 C1 O3 124.5(5) . . ?
O1 C1 H1 117.8 . . ?
O3 C1 H1 117.8 . . ?
N1 C3 H4 109.5 . . ?
N1 C3 H5 109.5 . . ?
H4 C3 H5 109.5 . . ?
N1 C3 H6 109.5 . . ?
H4 C3 H6 109.5 . . ?
H5 C3 H6 109.5 . . ?

_refine_diff_density_max         0.677
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.096

_shelx_res_file                  
;
TITL DMACuF_c1_p06_s_set2 in I2/a
    DMACuF_c1_p06_s_set2.res
    created by SHELXL-2016/6 at 10:17:44 on 17-Apr-2018
REM I2/a (#15 in standard setting)
CELL 0.41108  11.168524   8.470353   8.395552  90.0000  94.7845  90.0000
ZERR    4.00   0.000127   0.000256   0.000234   0.0000   0.0018   0.0000
LATT  2
SYMM -x+1/2, y,-z
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.13958!source kissel
DISP $H -0.00003  0.00000  0.64124!source kissel
DISP $N  0.00062  0.00099  7.18772!source kissel
DISP $O  0.00179  0.00182 10.15018!source kissel
DISP $Cu  0.24625  0.46844 1128.07893!source kissel
UNIT 20.00 44.00 4.00 24.00 4.00

OMIT -7 4 7
OMIT 13 2 5

L.S. 10
SIZE 0.06 0.04 0.03
ACTA
BOND $H
LIST 4
FMAP 2
RIGU C1 O1 O3
RIGU C2 O2
PLAN 20
WGHT    0.037500    3.917800
FVAR       2.80082
CU1   5    0.500000    0.500000    0.500000    10.50000    0.01944    0.04005 =
         0.02306   -0.00168   -0.00119    0.00107
O2    4    0.348785    0.615226    0.507935    11.00000    0.02121    0.04502 =
         0.03794   -0.00156    0.00004    0.00092

O1    4    0.422229    0.222257    0.114719    11.00000    0.03558    0.04728 =
         0.03270   -0.00798   -0.00371    0.00535
O3    4    0.436863    0.414680    0.291087    11.00000    0.03462    0.04972 =
         0.02660   -0.00687   -0.00512    0.00565
N1    3    0.250000    0.441175    0.000000    10.50000    0.03252    0.04924 =
         0.04348    0.00000   -0.00681    0.00000
DFIX H3 N1 1.0 0.1
H3    2    0.182695    0.388172   -0.040447    11.00000   -1.20000
C2    1    0.250000    0.546098    0.500000    10.50000    0.01942    0.03666 =
         0.03040    0.00000    0.00173    0.00000
AFIX  43
H2    2    0.250001    0.436303    0.500003    10.50000   -1.20000
AFIX   0
C1    1    0.466488    0.283695    0.240481    11.00000    0.02753    0.04486 =
         0.02895    0.00230   -0.00478    0.00021
AFIX  43
H1    2    0.525866    0.227842    0.300914    11.00000   -1.20000
AFIX   0
C3    1    0.187705    0.534527    0.110229    11.00000    0.04636    0.06962 =
         0.04450    0.00675    0.01593    0.00060
AFIX  33
H4    2    0.148126    0.465976    0.180260    11.00000   -1.20000
H5    2    0.244288    0.599923    0.172143    11.00000   -1.20000
H6    2    0.129165    0.599925    0.051778    11.00000   -1.20000
AFIX   0
HKLF 4




REM  DMACuF_c1_p06_s_set2 in I2/a
REM R1 =  0.0457 for     520 Fo > 4sig(Fo)  and  0.0630 for all     713 data
REM     65 parameters refined using     13 restraints

END

WGHT      0.0373      3.9182

REM Highest difference peak  0.677,  deepest hole -0.437,  1-sigma level  0.096
Q1    1   0.5110  0.5841  0.5912  11.00000  0.05    0.68
Q2    1   0.5081  0.4226  0.5843  11.00000  0.05    0.67
Q3    1   0.2500  0.5660  0.0000  10.50000  0.05    0.60
Q4    1   0.1482  0.3774  0.4920  11.00000  0.05    0.45
Q5    1   0.4411  0.5625  0.2796  11.00000  0.05    0.40
Q6    1   0.5814  0.5320  0.5639  11.00000  0.05    0.37
Q7    1   0.5733  0.2740  0.3767  11.00000  0.05    0.36
Q8    1   0.4954  0.3625  0.3536  11.00000  0.05    0.35
Q9    1   0.5079  0.1393  0.1507  11.00000  0.05    0.34
Q10   1   0.4989  0.3555  0.4925  11.00000  0.05    0.32
Q11   1   0.4697  0.4826  0.3343  11.00000  0.05    0.32
Q12   1   0.6525  0.2081  0.3670  11.00000  0.05    0.30
Q13   1   0.3670  0.5590  0.3815  11.00000  0.05    0.30
Q14   1   0.4868  0.5018  0.2528  11.00000  0.05    0.28
Q15   1   0.2768  0.5011  0.0914  11.00000  0.05    0.27
Q16   1   0.4175  0.4975  0.2025  11.00000  0.05    0.27
Q17   1   0.3522  0.5600  0.5782  11.00000  0.05    0.27
Q18   1   0.3315  0.7116  0.5585  11.00000  0.05    0.27
Q19   1   0.5798  0.5807  0.4716  11.00000  0.05    0.27
Q20   1   0.4194  0.2872  0.1697  11.00000  0.05    0.26
;
_shelx_res_checksum              13842
####################################################################### 
# 
# 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_DMAFeF_c6_p01_s
_database_code_depnum_ccdc_archive 'CCDC 1837760'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Fe N O6'
_chemical_formula_weight         237.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1965 0.3053 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   7.9947(2)
_cell_length_b                   7.9947(2)
_cell_length_c                   20.7241(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1147.11(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    367
_cell_measurement_theta_min      2.0470
_cell_measurement_theta_max      18.8540

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.440
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58750
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_pressure         '5.50 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41119
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            999
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.047
_diffrn_reflns_theta_max         19.474
_diffrn_reflns_theta_full        14.283
_diffrn_measured_fraction_theta_max 0.675
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.675
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.675
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             389
_reflns_number_gt                337
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+3.4704P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         388
_refine_ls_number_parameters     31
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1074
_refine_ls_wR_factor_gt          0.1030
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.191
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.666667 0.333333 0.333333 0.0237(3) Uani 1 6 d S T P . .
N1 N 0.7426(13) 0.333333 0.083333 0.042(2) Uani 0.3333 2 d DS T P . .
H3 H 0.779(8) 0.246(8) 0.075(6) 0.050 Uiso 0.3333 1 d D U P . .
C2 C 0.666667 0.333333 0.0255(3) 0.0629(19) Uani 1 3 d DS T P . .
H2 H 0.576(6) 0.206(5) 0.010(3) 0.075 Uiso 1 1 d D U . . .
O1 O 0.8644(3) 0.3008(3) 0.27729(9) 0.0354(5) Uani 1 1 d . . . . .
C1 C 1.000000 0.4418(4) 0.250000 0.0297(6) Uani 1 2 d S T P . .
H1 H 1.000003 0.558130 0.250002 0.036 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0242(3) 0.0242(3) 0.0226(4) 0.000 0.000 0.01212(17)
N1 0.035(3) 0.030(4) 0.059(7) -0.017(4) -0.008(2) 0.015(2)
C2 0.081(3) 0.081(3) 0.027(2) 0.000 0.000 0.0405(16)
O1 0.0335(8) 0.0338(9) 0.0377(10) 0.0030(7) 0.0104(7) 0.0161(7)
C1 0.0288(14) 0.0300(11) 0.0299(14) 0.0014(5) 0.0029(11) 0.0144(7)

_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
Fe1 O1 2.0797(17) 31_655 ?
Fe1 O1 2.0798(17) 33_545 ?
Fe1 O1 2.0798(17) 3_665 ?
Fe1 O1 2.0798(17) 32 ?
Fe1 O1 2.0798(17) 2_655 ?
Fe1 O1 2.0798(17) . ?
N1 N1 1.052(18) 3_665 ?
N1 N1 1.052(18) 2_655 ?
N1 C2 1.344(7) 16_544 ?
N1 C2 1.344(7) . ?
O1 C1 1.243(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 Fe1 O1 91.85(8) 31_655 33_545 ?
O1 Fe1 O1 88.15(8) 31_655 3_665 ?
O1 Fe1 O1 180.0 33_545 3_665 ?
O1 Fe1 O1 91.85(8) 31_655 32 ?
O1 Fe1 O1 91.85(8) 33_545 32 ?
O1 Fe1 O1 88.15(8) 3_665 32 ?
O1 Fe1 O1 88.15(8) 31_655 2_655 ?
O1 Fe1 O1 88.15(8) 33_545 2_655 ?
O1 Fe1 O1 91.85(8) 3_665 2_655 ?
O1 Fe1 O1 180.0 32 2_655 ?
O1 Fe1 O1 180.0 31_655 . ?
O1 Fe1 O1 88.15(8) 33_545 . ?
O1 Fe1 O1 91.84(8) 3_665 . ?
O1 Fe1 O1 88.15(8) 32 . ?
O1 Fe1 O1 91.84(8) 2_655 . ?
N1 N1 N1 59.998(1) 3_665 2_655 ?
N1 N1 C2 67.0(3) 3_665 16_544 ?
N1 N1 C2 67.0(3) 2_655 16_544 ?
N1 N1 C2 67.0(3) 3_665 . ?
N1 N1 C2 67.0(3) 2_655 . ?
C2 N1 C2 126.3(8) 16_544 . ?
N1 C2 N1 46.0(7) . 3_665 ?
N1 C2 N1 46.0(7) . 2_655 ?
N1 C2 N1 46.0(7) 3_665 2_655 ?
C1 O1 Fe1 120.92(17) . . ?
O1 C1 O1 123.8(3) . 6_765 ?

_refine_diff_density_max         0.385
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.091

_shelx_res_file                  
;
TITL DMAFeF_c6_p01_s in R-3c
    DMAFeF_c6_p01_s.res
    created by SHELXL-2016/6 at 17:17:18 on 22-Mar-2018
REM R-3c (#167 in standard setting)
CELL 0.41119   7.994657   7.994657  20.724113  90.0000  90.0000 120.0000
ZERR    6.00   0.000203   0.000203   0.000544   0.0000   0.0000   0.0000
LATT  3
SYMM -y, x-y, z
SYMM -x+y,-x, z
SYMM  y, x,-z+1/2
SYMM  x-y,-y,-z+1/2
SYMM -x,-x+y,-z+1/2
SFAC C H N O Fe
DISP $C -0.00006  0.00048  5.13891!source kissel
DISP $H -0.00003  0.00000  0.64123!source kissel
DISP $N  0.00062  0.00099  7.18643!source kissel
DISP $O  0.00179  0.00182 10.14789!source kissel
DISP $Fe  0.19654  0.30533 739.74304!source kissel
UNIT 30.00 66.00 6.00 36.00 6.00
OMIT 0 1 2
OMIT -2 2 8
OMIT -1 1 4
OMIT -1   2   0
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 10
ACTA
BOND
RIGU C1 O1
EQIV $3 1-x+y, 1-x, +z
EQIV $1 1/3+x-y, 2/3-y, 1/6-z
FMAP 2
PLAN 20
WGHT    0.042200    3.470400
FVAR       3.57337
MOLE   1
FE1   5    0.666667    0.333333    0.333333    10.16667    0.02423    0.02423 =
         0.02256    0.00000    0.00000    0.01212
N1    3    0.742603    0.333333    0.083333    10.16667    0.03460    0.03014 =
         0.05852   -0.01686   -0.00843    0.01507
DFIX 0.9 0.01 N1 H3
DFIX 1.2 0.1 H3 H3_$1
H3    2    0.779255    0.246131    0.074594    10.33333   -1.20000
C2    1    0.666667    0.333333    0.025450    10.33333    0.08096    0.08096 =
         0.02680    0.00000    0.00000    0.04048
DFIX 1.1 0.1 C2 H2
DFIX 1.5 0.1 H2 H2_$3
H2    2    0.576284    0.206072    0.010253    11.00000   -1.20000
O1    4    0.864355    0.300805    0.277288    11.00000    0.03353    0.03384 =
         0.03774    0.00303    0.01038    0.01609
C1    1    1.000000    0.441801    0.250000    10.50000    0.02879    0.03000 =
         0.02989    0.00144    0.00288    0.01439
AFIX  43
H1    2    1.000003    0.558130    0.250002    10.50000   -1.20000
MOLE   2
MOLE   3
REM #####
REM #####
REM #####
AFIX   0
HKLF 4




REM  DMAFeF_c6_p01_s in R-3c
REM R1 =  0.0377 for     336 Fo > 4sig(Fo)  and  0.0419 for all     388 data
REM     31 parameters refined using      7 restraints

END

WGHT      0.0370      3.5010

REM Highest difference peak  0.385,  deepest hole -0.497,  1-sigma level  0.091
Q1    1   0.8259  0.3332  0.2513  11.00000  0.05    0.39
Q2    1   0.6667  0.3333  0.3755  10.33333  0.05    0.38
Q3    1   0.8038  0.3479  0.2974  11.00000  0.05    0.37
Q4    1   0.6667  0.3333 -0.0153  10.33333  0.05    0.36
Q5    1   0.7223  0.2963  0.2668  11.00000  0.05    0.34
Q6    1   0.6289  0.2358  0.3484  11.00000  0.05    0.32
Q7    1   0.6930  0.4616  0.3632  11.00000  0.05    0.27
Q8    1   0.9016  0.3866  0.2903  11.00000  0.05    0.25
Q9    1   1.0115  0.6256  0.3179  11.00000  0.05    0.25
Q10   1   1.0315  0.5767  0.2808  11.00000  0.05    0.24
Q11   1   0.7381  0.1828  0.3248  11.00000  0.05    0.24
Q12   1   0.4816  0.2386  0.0127  11.00000  0.05    0.24
Q13   1   0.8647  0.2959  0.3158  11.00000  0.05    0.24
Q14   1   1.2004  0.6699  0.2572  11.00000  0.05    0.23
Q15   1   0.8806  0.5249  0.2750  11.00000  0.05    0.23
Q16   1   1.0901  0.7073  0.2798  11.00000  0.05    0.22
Q17   1   0.9736  0.4872  0.3218  11.00000  0.05    0.21
Q18   1   0.9849  0.3783  0.3125  11.00000  0.05    0.20
Q19   1   0.6586  0.2454 -0.0249  11.00000  0.05    0.18
Q20   1   0.8452  0.2146  0.2477  11.00000  0.05    0.18
;
_shelx_res_checksum              33980

# start Validation Reply Form
_vrf_PLAT413_DMAFeF_c6_p01_s     
;
PROBLEM: Short Inter XH3 .. XHn     H2       ..H2               1.57 Ang.  
RESPONSE: The H atoms are only restrained by distance and angle restraints
and as the (CH3)2NH2 unit is dynamically disordered, accurate positioning
of the H atoms may not always be possible.
;
_vrf_PLAT415_DMAFeF_c6_p01_s     
;
PROBLEM: Short Inter D-H..H-X       H2       ..H3               1.64 Ang.  
RESPONSE: The H2 belongs to the CH3 unit and the H3 to the NH2 unit of the 
(CH3)2NH2 unit. As they are part of the same molecular unit, it is likely
that they have close H...H distances. 
;
_vrf_PLAT029_DMAFeF_c6_p01_s     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.961 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_DMAFeF_c6_p01_s     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          7 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT978_DMAFeF_c6_p01_s     
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_DMACuF_c2_p10
_database_code_depnum_ccdc_archive 'CCDC 1837745'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c2_p10       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.543 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT043_DMACuF_c2_p10       
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      11.08 Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT911_DMACuF_c2_p10       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        311 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_CHEMW03_DMACuF_c2_p10       
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT041_DMACuF_c2_p10       
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT068_DMACuF_c2_p10       
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT155_DMACuF_c2_p10       
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The cell was kept in the given setting so as to be more comparable to the ambient phase unit cell.
;
_vrf_PLAT202_DMACuF_c2_p10       
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check
RESPONSE: Due to the many parameters in the refinement, refinement of isotropic thermal parameters were preferred.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4687 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.4239(8)
_cell_length_b                   5.9107(12)
_cell_length_c                   5.755(5)
_cell_angle_alpha                95.38(4)
_cell_angle_beta                 89.33(4)
_cell_angle_gamma                96.927(15)
_cell_volume                     182.33(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    99
_cell_measurement_theta_min      2.1890
_cell_measurement_theta_max      13.8370

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.228
_exptl_crystal_F_000             125
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.675
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.29228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '6.77 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            652
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.188
_diffrn_reflns_theta_max         19.543
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.372
_diffrn_measured_fraction_theta_full 0.543
_diffrn_reflns_Laue_measured_fraction_max 0.372
_diffrn_reflns_Laue_measured_fraction_full 0.543
_diffrn_reflns_point_group_measured_fraction_max 0.372
_diffrn_reflns_point_group_measured_fraction_full 0.543
_reflns_number_total             652
_reflns_number_gt                397
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1275P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         652
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.2012
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0315(7) Uani 1 2 d S . P . .
O1 O 0.6337(19) 0.643(3) 0.803(2) 0.033(3) Uiso 0.5 1 d . . P . .
O2 O 0.7026(18) 0.588(3) 1.167(2) 0.031(3) Uiso 0.5 1 d . . P . .
O3 O -0.1878(17) 0.609(3) 0.355(2) 0.025(2) Uiso 0.5 1 d . . P . .
O4 O 0.217(2) 0.603(3) 0.362(2) 0.034(3) Uiso 0.5 1 d . . P . .
O5 O 0.338(2) -0.182(4) 0.400(3) 0.042(3) Uiso 0.5 1 d . . P . .
O6 O 0.370(2) 0.189(3) 0.389(3) 0.043(3) Uiso 0.5 1 d . . P . .
C1 C 0.585(2) 0.535(3) 0.980(3) 0.020(3) Uiso 0.5 1 d . . P . .
C3 C 0.435(2) 0.005(5) 0.460(3) 0.031(4) Uiso 0.5 1 d . . P . .
C2 C 0.007(2) 0.547(3) 0.440(2) 0.018(3) Uiso 0.5 1 d . . P . .
C4 C 0.165(2) -0.102(3) 0.931(3) 0.066(3) Uiso 1 1 d . . . . .
N1 N -0.002(3) -0.014(4) 1.084(3) 0.036(3) Uiso 0.5 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0248(8) 0.0388(15) 0.0264(9) -0.0094(11) -0.0075(5) -0.0059(7)

_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
Cu1 O4 1.922(12) 2_666 ?
Cu1 O4 1.922(12) . ?
Cu1 O6 1.942(19) . ?
Cu1 O6 1.942(19) 2_666 ?
Cu1 O3 1.945(11) 2_566 ?
Cu1 O3 1.945(11) 1_655 ?
Cu1 O1 1.974(14) 2_666 ?
Cu1 O1 1.974(14) . ?
Cu1 O2 2.269(13) 2_667 ?
Cu1 O2 2.269(13) 1_554 ?
Cu1 O5 2.293(19) 1_565 ?
Cu1 O5 2.293(19) 2_656 ?
O1 C1 1.26(2) . ?
O1 O6 1.56(2) 2_666 ?
O2 O3 1.228(18) 1_656 ?
O2 C1 1.25(2) . ?
O2 C1 1.823(18) 2_667 ?
O3 C2 1.276(18) . ?
O3 C2 1.913(18) 2_566 ?
O4 C2 1.238(19) . ?
O4 O5 1.36(3) 1_565 ?
O4 C2 1.862(18) 2_566 ?
O5 C3 1.19(3) . ?
O5 C3 1.68(3) 2_656 ?
O6 C3 1.28(3) . ?
O6 C3 1.92(3) 2_656 ?
C1 C1 1.00(3) 2_667 ?
C3 C3 0.86(3) 2_656 ?
C2 C2 0.93(3) 2_566 ?
C4 N1 1.20(2) 2_557 ?
C4 N1 1.37(2) . ?
N1 N1 0.99(3) 2_557 ?

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
O4 Cu1 O4 180.0 2_666 . ?
O4 Cu1 O6 91.5(7) 2_666 . ?
O4 Cu1 O6 88.5(7) . . ?
O4 Cu1 O6 88.5(7) 2_666 2_666 ?
O4 Cu1 O6 91.5(7) . 2_666 ?
O6 Cu1 O6 180.0(5) . 2_666 ?
O4 Cu1 O3 112.9(6) 2_666 2_566 ?
O4 Cu1 O3 67.1(6) . 2_566 ?
O6 Cu1 O3 66.2(6) . 2_566 ?
O6 Cu1 O3 113.8(6) 2_666 2_566 ?
O4 Cu1 O3 67.1(6) 2_666 1_655 ?
O4 Cu1 O3 112.9(6) . 1_655 ?
O6 Cu1 O3 113.8(6) . 1_655 ?
O6 Cu1 O3 66.2(6) 2_666 1_655 ?
O3 Cu1 O3 180.0 2_566 1_655 ?
O4 Cu1 O1 121.0(6) 2_666 2_666 ?
O4 Cu1 O1 59.0(6) . 2_666 ?
O6 Cu1 O1 46.9(7) . 2_666 ?
O6 Cu1 O1 133.1(7) 2_666 2_666 ?
O3 Cu1 O1 88.9(5) 2_566 2_666 ?
O3 Cu1 O1 91.1(5) 1_655 2_666 ?
O4 Cu1 O1 59.0(6) 2_666 . ?
O4 Cu1 O1 121.0(6) . . ?
O6 Cu1 O1 133.1(7) . . ?
O6 Cu1 O1 46.9(7) 2_666 . ?
O3 Cu1 O1 91.1(5) 2_566 . ?
O3 Cu1 O1 88.9(5) 1_655 . ?
O1 Cu1 O1 180.0 2_666 . ?
O4 Cu1 O2 85.5(5) 2_666 2_667 ?
O4 Cu1 O2 94.5(5) . 2_667 ?
O6 Cu1 O2 83.3(6) . 2_667 ?
O6 Cu1 O2 96.7(6) 2_666 2_667 ?
O3 Cu1 O2 32.7(5) 2_566 2_667 ?
O3 Cu1 O2 147.3(5) 1_655 2_667 ?
O1 Cu1 O2 119.3(5) 2_666 2_667 ?
O1 Cu1 O2 60.7(5) . 2_667 ?
O4 Cu1 O2 94.5(5) 2_666 1_554 ?
O4 Cu1 O2 85.5(5) . 1_554 ?
O6 Cu1 O2 96.7(6) . 1_554 ?
O6 Cu1 O2 83.3(6) 2_666 1_554 ?
O3 Cu1 O2 147.3(5) 2_566 1_554 ?
O3 Cu1 O2 32.7(5) 1_655 1_554 ?
O1 Cu1 O2 60.7(5) 2_666 1_554 ?
O1 Cu1 O2 119.3(5) . 1_554 ?
O2 Cu1 O2 180.0 2_667 1_554 ?
O4 Cu1 O5 143.7(6) 2_666 1_565 ?
O4 Cu1 O5 36.3(6) . 1_565 ?
O6 Cu1 O5 124.0(6) . 1_565 ?
O6 Cu1 O5 56.0(6) 2_666 1_565 ?
O3 Cu1 O5 90.8(5) 2_566 1_565 ?
O3 Cu1 O5 89.2(5) 1_655 1_565 ?
O1 Cu1 O5 84.8(6) 2_666 1_565 ?
O1 Cu1 O5 95.2(6) . 1_565 ?
O2 Cu1 O5 104.4(5) 2_667 1_565 ?
O2 Cu1 O5 75.6(5) 1_554 1_565 ?
O4 Cu1 O5 36.3(6) 2_666 2_656 ?
O4 Cu1 O5 143.7(6) . 2_656 ?
O6 Cu1 O5 56.0(6) . 2_656 ?
O6 Cu1 O5 124.0(6) 2_666 2_656 ?
O3 Cu1 O5 89.2(5) 2_566 2_656 ?
O3 Cu1 O5 90.8(5) 1_655 2_656 ?
O1 Cu1 O5 95.2(6) 2_666 2_656 ?
O1 Cu1 O5 84.8(6) . 2_656 ?
O2 Cu1 O5 75.6(5) 2_667 2_656 ?
O2 Cu1 O5 104.4(5) 1_554 2_656 ?
O5 Cu1 O5 180.0(8) 1_565 2_656 ?
C1 O1 O6 163.8(14) . 2_666 ?
C1 O1 Cu1 117.6(12) . . ?
O6 O1 Cu1 65.5(8) 2_666 . ?
O3 O2 C1 171(2) 1_656 . ?
O3 O2 C1 143.5(12) 1_656 2_667 ?
C1 O2 C1 31.3(12) . 2_667 ?
O3 O2 Cu1 59.0(8) 1_656 1_556 ?
C1 O2 Cu1 116.6(10) . 1_556 ?
C1 O2 Cu1 85.3(6) 2_667 1_556 ?
O2 O3 C2 138.4(14) 1_454 . ?
O2 O3 C2 144.0(16) 1_454 2_566 ?
C2 O3 C2 24.9(10) . 2_566 ?
O2 O3 Cu1 88.3(8) 1_454 1_455 ?
C2 O3 Cu1 115.8(10) . 1_455 ?
C2 O3 Cu1 90.9(8) 2_566 1_455 ?
C2 O4 O5 122.8(18) . 1_565 ?
C2 O4 C2 26.1(11) . 2_566 ?
O5 O4 C2 127.3(13) 1_565 2_566 ?
C2 O4 Cu1 119.4(12) . . ?
O5 O4 Cu1 86.9(8) 1_565 . ?
C2 O4 Cu1 93.3(8) 2_566 . ?
C3 O5 O4 172(2) . 1_545 ?
C3 O5 C3 29.1(17) . 2_656 ?
O4 O5 C3 147.8(14) 1_545 2_656 ?
C3 O5 Cu1 121.2(14) . 1_545 ?
O4 O5 Cu1 56.8(10) 1_545 1_545 ?
C3 O5 Cu1 92.1(8) 2_656 1_545 ?
C3 O6 O1 150.4(16) . 2_666 ?
C3 O6 C3 21.2(15) . 2_656 ?
O1 O6 C3 145.6(10) 2_666 2_656 ?
C3 O6 Cu1 126.3(13) . . ?
O1 O6 Cu1 67.6(9) 2_666 . ?
C3 O6 Cu1 105.7(9) 2_656 . ?
C1 C1 O2 108(2) 2_667 . ?
C1 C1 O1 123(2) 2_667 . ?
O2 C1 O1 121.4(16) . . ?
C1 C1 O2 40.8(16) 2_667 2_667 ?
O2 C1 O2 148.7(11) . 2_667 ?
O1 C1 O2 86.8(10) . 2_667 ?
C3 C3 O5 109(4) 2_656 . ?
C3 C3 O6 126(4) 2_656 . ?
O5 C3 O6 124.2(17) . . ?
C3 C3 O5 42(3) 2_656 2_656 ?
O5 C3 O5 150.9(17) . 2_656 ?
O6 C3 O5 84.7(15) . 2_656 ?
C3 C3 O6 32(3) 2_656 2_656 ?
O5 C3 O6 76.7(17) . 2_656 ?
O6 C3 O6 158.8(15) . 2_656 ?
O5 C3 O6 74.2(9) 2_656 2_656 ?
C2 C2 O4 118(2) 2_566 . ?
C2 C2 O3 119.7(19) 2_566 . ?
O4 C2 O3 122.4(14) . . ?
C2 C2 O4 36.0(13) 2_566 2_566 ?
O4 C2 O4 153.9(11) . 2_566 ?
O3 C2 O4 83.7(9) . 2_566 ?
C2 C2 O3 35.4(13) 2_566 2_566 ?
O4 C2 O3 82.5(10) . 2_566 ?
O3 C2 O3 155.1(10) . 2_566 ?
O4 C2 O3 71.4(8) 2_566 2_566 ?
N1 C4 N1 44.9(15) 2_557 . ?
N1 N1 C4 77(2) 2_557 2_557 ?
N1 N1 C4 58(2) 2_557 . ?
C4 N1 C4 135.1(15) 2_557 . ?

_refine_diff_density_max         0.967
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.155

_shelx_res_file                  
;
TITL DMACuF_c2_p10_s_twin in P-1
    DMACuF_c2_p10_s_mask1p5_twin1_hklf5.res
    created by SHELXL-2016/6 at 16:24:51 on 21-Mar-2018
REM P-1 (#2 in standard setting)
CELL 0.41108  5.423927 5.910736  5.754539  95.3833  89.3255   96.9266
ZERR    1.00  0.000846 0.001169  0.004892  0.0449   0.0370    0.0145
LATT  1
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.14091!source kissel
DISP $H -0.00003  0.00000  0.64127!source kissel
DISP $N  0.00062  0.00099  7.19030!source kissel
DISP $O  0.00180  0.00183 10.15475!source kissel
DISP $Cu  0.24634  0.46870 1129.00277!source kissel
UNIT 5.00 11.00 1.00 6.00 1.00
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 50
SIZE 0.11 0.05 0.03
ACTA
BOND
FMAP 2
PLAN 20
MERG 0
WGHT    0.127500
BASF   0.59257
FVAR      22.09062
MOLE   1
CU1   5    0.500000    0.500000    0.500000    10.50000    0.02478    0.03878 =
         0.02639   -0.00940   -0.00750   -0.00594
O1    4    0.633668    0.643106    0.803497    10.50000    0.03306
O2    4    0.702619    0.588004    1.167093    10.50000    0.03124
O3    4   -0.187821    0.608737    0.354760    10.50000    0.02522
O4    4    0.217366    0.602935    0.362194    10.50000    0.03358
O5    4    0.337843   -0.181556    0.400236    10.50000    0.04229
O6    4    0.370159    0.188507    0.388920    10.50000    0.04325
C1    1    0.585068    0.534685    0.980352    10.50000    0.02042
C3    1    0.434789    0.005362    0.459657    10.50000    0.03120
C2    1    0.007111    0.547237    0.439726    10.50000    0.01806
C4    1    0.165462   -0.102310    0.930835    11.00000    0.06570
N1    3   -0.001889   -0.014475    1.083735    10.50000    0.03617
MOLE   2
HKLF 5 1 0 1 0 1 0 0 0 0 1 1 0




REM  DMACuF_c2_p10_s_twin in P-1
REM R1 =  0.0732 for     397 Fo > 4sig(Fo)  and  0.1061 for all     652 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.1275      0.0000

REM Highest difference peak  0.967,  deepest hole -1.022,  1-sigma level  0.155
Q1    1   0.3583  0.5108  0.5096  11.00000  0.05    0.97
Q2    1  -0.2699  0.6360  0.5172  11.00000  0.05    0.87
Q3    1   0.4874  0.3088  0.4794  11.00000  0.05    0.72
Q4    1   0.1417 -0.0375  0.8483  11.00000  0.05    0.71
Q5    1   0.1798 -0.1987  0.9779  11.00000  0.05    0.67
Q6    1   0.4939  0.5223  0.8139  11.00000  0.05    0.56
Q7    1   0.5038  0.5126  0.7066  11.00000  0.05    0.51
Q8    1   0.1996  0.5228  0.4366  11.00000  0.05    0.48
Q9    1   0.4865  0.2063  0.4623  11.00000  0.05    0.46
Q10   1   0.7286  0.5265  1.1857  11.00000  0.05    0.45
Q11   1   0.3594  0.5158  0.3194  11.00000  0.05    0.44
Q12   1   0.4704  0.3466  0.6159  11.00000  0.05    0.43
Q13   1   0.1815  0.2239  0.4441  11.00000  0.05    0.39
Q14   1   0.0101 -0.0811  1.1247  11.00000  0.05    0.38
Q15   1   0.5840 -0.0366  0.3278  11.00000  0.05    0.37
Q16   1   0.3679  0.5285  0.6615  11.00000  0.05    0.36
Q17   1   0.8766  0.4790  0.9844  11.00000  0.05    0.35
Q18   1   0.4024 -0.0036  0.3825  11.00000  0.05    0.35
Q19   1  -0.2061  0.4030  0.3337  11.00000  0.05    0.35
Q20   1   0.7068  0.5306  0.7774  11.00000  0.05    0.34
;
_shelx_res_checksum              56172
####################################################################### 
# 
# 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_DMACuF_c2_p11
_database_code_depnum_ccdc_archive 'CCDC 1837746'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_DMACuF_c2_p11       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.538 Why?
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT043_DMACuF_c2_p11       
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      11.08 Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_CHEMW03_DMACuF_c2_p11       
;
PROBLEM: The ratio of given/expected molecular weight as
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT041_DMACuF_c2_p11       
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT068_DMACuF_c2_p11       
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)...     Please Check
RESPONSE: The hydrogen atoms were excluded from the refinement.
;
_vrf_PLAT155_DMACuF_c2_p11       
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do !
RESPONSE: The cell was kept in the given setting so as to be more comparable to the ambient phase unit cell.
;
_vrf_PLAT202_DMACuF_c2_p11       
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check
RESPONSE: Due to the many parameters in the refinement, refinement of isotropic thermal parameters were preffered.
;
# Added during the CSD deposition process: Tuesday 17 April 2018 09:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Cu O6, C2 H8 N'
_chemical_formula_sum            'C5 H11 Cu N O6'
_chemical_formula_weight         244.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.2463 0.4687 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.3901(9)
_cell_length_b                   5.8969(14)
_cell_length_c                   5.720(4)
_cell_angle_alpha                95.95(5)
_cell_angle_beta                 88.82(4)
_cell_angle_gamma                96.958(16)
_cell_volume                     179.49(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    121
_cell_measurement_theta_min      2.2010
_cell_measurement_theta_max      14.1380

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.264
_exptl_crystal_F_000             125
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.685
_shelx_estimated_absorpt_T_min   0.954
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.19374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '7.54 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41108
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            632
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.202
_diffrn_reflns_theta_max         19.599
_diffrn_reflns_theta_full        14.279
_diffrn_measured_fraction_theta_max 0.369
_diffrn_measured_fraction_theta_full 0.538
_diffrn_reflns_Laue_measured_fraction_max 0.369
_diffrn_reflns_Laue_measured_fraction_full 0.538
_diffrn_reflns_point_group_measured_fraction_max 0.369
_diffrn_reflns_point_group_measured_fraction_full 0.538
_reflns_number_total             632
_reflns_number_gt                414
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1356P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         632
_refine_ls_number_parameters     52
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0743
_refine_ls_wR_factor_ref         0.2072
_refine_ls_wR_factor_gt          0.1968
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Cu1 Cu 0.500000 0.500000 0.500000 0.0312(7) Uani 1 2 d S . P . .
O1 O 0.6390(19) 0.640(3) 0.802(2) 0.031(3) Uiso 0.5 1 d . . P . .
O2 O 0.7105(19) 0.581(3) 1.165(3) 0.033(3) Uiso 0.5 1 d . . P . .
O3 O -0.1881(19) 0.607(3) 0.354(3) 0.031(3) Uiso 0.5 1 d . . P . .
O4 O 0.220(2) 0.606(3) 0.358(3) 0.032(3) Uiso 0.5 1 d . . P . .
O5 O 0.334(2) -0.186(4) 0.407(3) 0.041(3) Uiso 0.5 1 d . . P . .
O6 O 0.367(2) 0.185(3) 0.388(3) 0.045(3) Uiso 0.5 1 d . . P . .
C1 C 0.589(2) 0.536(3) 0.979(3) 0.022(3) Uiso 0.5 1 d . . P . .
C3 C 0.434(3) 0.007(5) 0.460(3) 0.035(4) Uiso 0.5 1 d . . P . .
C2 C 0.005(2) 0.547(3) 0.439(2) 0.016(3) Uiso 0.5 1 d . . P . .
C4 C 0.170(2) -0.100(3) 0.938(3) 0.064(3) Uiso 1 1 d . . . . .
N1 N -0.002(3) -0.016(4) 1.089(3) 0.038(3) Uiso 0.5 1 d . . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0240(7) 0.0389(14) 0.0265(9) -0.0081(11) -0.0080(5) -0.0051(7)

_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
Cu1 O4 1.926(12) . ?
Cu1 O4 1.926(12) 2_666 ?
Cu1 O3 1.928(12) 2_566 ?
Cu1 O3 1.928(12) 1_655 ?
Cu1 O6 1.955(19) . ?
Cu1 O6 1.955(19) 2_666 ?
Cu1 O1 1.960(13) 2_666 ?
Cu1 O1 1.960(13) . ?
Cu1 O5 2.268(19) 2_656 ?
Cu1 O5 2.268(19) 1_565 ?
Cu1 O2 2.272(14) 2_667 ?
Cu1 O2 2.272(14) 1_554 ?
O1 C1 1.25(2) . ?
O1 O6 1.58(2) 2_666 ?
O2 O3 1.21(2) 1_656 ?
O2 C1 1.24(2) . ?
O2 C1 1.855(18) 2_667 ?
O3 C2 1.262(18) . ?
O3 C2 1.922(18) 2_566 ?
O4 C2 1.260(19) . ?
O4 O5 1.31(3) 1_565 ?
O4 C2 1.879(18) 2_566 ?
O5 C3 1.21(3) . ?
O5 C3 1.68(3) 2_656 ?
O6 C3 1.26(3) . ?
C1 C1 1.04(3) 2_667 ?
C3 C3 0.87(3) 2_656 ?
C2 C2 0.93(3) 2_566 ?
C4 N1 1.22(2) 2_557 ?
C4 N1 1.36(2) . ?
N1 N1 1.05(4) 2_557 ?

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
O4 Cu1 O4 180.0 . 2_666 ?
O4 Cu1 O3 68.3(6) . 2_566 ?
O4 Cu1 O3 111.7(6) 2_666 2_566 ?
O4 Cu1 O3 111.7(6) . 1_655 ?
O4 Cu1 O3 68.3(6) 2_666 1_655 ?
O3 Cu1 O3 180.0 2_566 1_655 ?
O4 Cu1 O6 89.0(7) . . ?
O4 Cu1 O6 91.0(7) 2_666 . ?
O3 Cu1 O6 65.9(7) 2_566 . ?
O3 Cu1 O6 114.1(7) 1_655 . ?
O4 Cu1 O6 91.0(7) . 2_666 ?
O4 Cu1 O6 89.0(7) 2_666 2_666 ?
O3 Cu1 O6 114.1(7) 2_566 2_666 ?
O3 Cu1 O6 65.9(7) 1_655 2_666 ?
O6 Cu1 O6 180.0 . 2_666 ?
O4 Cu1 O1 57.5(6) . 2_666 ?
O4 Cu1 O1 122.5(6) 2_666 2_666 ?
O3 Cu1 O1 88.2(5) 2_566 2_666 ?
O3 Cu1 O1 91.8(5) 1_655 2_666 ?
O6 Cu1 O1 47.5(7) . 2_666 ?
O6 Cu1 O1 132.5(7) 2_666 2_666 ?
O4 Cu1 O1 122.5(6) . . ?
O4 Cu1 O1 57.5(6) 2_666 . ?
O3 Cu1 O1 91.8(5) 2_566 . ?
O3 Cu1 O1 88.2(5) 1_655 . ?
O6 Cu1 O1 132.5(7) . . ?
O6 Cu1 O1 47.5(7) 2_666 . ?
O1 Cu1 O1 180.0 2_666 . ?
O4 Cu1 O5 144.9(6) . 2_656 ?
O4 Cu1 O5 35.1(6) 2_666 2_656 ?
O3 Cu1 O5 90.1(6) 2_566 2_656 ?
O3 Cu1 O5 89.9(6) 1_655 2_656 ?
O6 Cu1 O5 56.3(6) . 2_656 ?
O6 Cu1 O5 123.7(6) 2_666 2_656 ?
O1 Cu1 O5 96.0(6) 2_666 2_656 ?
O1 Cu1 O5 84.0(6) . 2_656 ?
O4 Cu1 O5 35.1(6) . 1_565 ?
O4 Cu1 O5 144.9(6) 2_666 1_565 ?
O3 Cu1 O5 89.9(6) 2_566 1_565 ?
O3 Cu1 O5 90.1(6) 1_655 1_565 ?
O6 Cu1 O5 123.7(6) . 1_565 ?
O6 Cu1 O5 56.3(6) 2_666 1_565 ?
O1 Cu1 O5 84.0(6) 2_666 1_565 ?
O1 Cu1 O5 96.0(6) . 1_565 ?
O5 Cu1 O5 180.0 2_656 1_565 ?
O4 Cu1 O2 94.5(5) . 2_667 ?
O4 Cu1 O2 85.5(5) 2_666 2_667 ?
O3 Cu1 O2 32.2(5) 2_566 2_667 ?
O3 Cu1 O2 147.8(5) 1_655 2_667 ?
O6 Cu1 O2 83.5(7) . 2_667 ?
O6 Cu1 O2 96.5(7) 2_666 2_667 ?
O1 Cu1 O2 118.7(5) 2_666 2_667 ?
O1 Cu1 O2 61.3(5) . 2_667 ?
O5 Cu1 O2 77.6(5) 2_656 2_667 ?
O5 Cu1 O2 102.4(5) 1_565 2_667 ?
O4 Cu1 O2 85.5(5) . 1_554 ?
O4 Cu1 O2 94.5(5) 2_666 1_554 ?
O3 Cu1 O2 147.8(5) 2_566 1_554 ?
O3 Cu1 O2 32.2(5) 1_655 1_554 ?
O6 Cu1 O2 96.5(7) . 1_554 ?
O6 Cu1 O2 83.5(7) 2_666 1_554 ?
O1 Cu1 O2 61.3(5) 2_666 1_554 ?
O1 Cu1 O2 118.7(5) . 1_554 ?
O5 Cu1 O2 102.4(5) 2_656 1_554 ?
O5 Cu1 O2 77.6(5) 1_565 1_554 ?
O2 Cu1 O2 180.0 2_667 1_554 ?
C1 O1 O6 161.8(14) . 2_666 ?
C1 O1 Cu1 118.2(12) . . ?
O6 O1 Cu1 66.0(8) 2_666 . ?
O3 O2 C1 173(2) 1_656 . ?
O3 O2 C1 141.7(13) 1_656 2_667 ?
C1 O2 C1 32.2(12) . 2_667 ?
O3 O2 Cu1 58.1(9) 1_656 1_556 ?
C1 O2 Cu1 116.1(11) . 1_556 ?
C1 O2 Cu1 83.9(6) 2_667 1_556 ?
O2 O3 C2 136.3(15) 1_454 . ?
O2 O3 C2 142.3(17) 1_454 2_566 ?
C2 O3 C2 24.5(10) . 2_566 ?
O2 O3 Cu1 89.7(9) 1_454 1_455 ?
C2 O3 Cu1 115.6(11) . 1_455 ?
C2 O3 Cu1 91.1(8) 2_566 1_455 ?
C2 O4 O5 121.5(18) . 1_565 ?
C2 O4 C2 26.3(10) . 2_566 ?
O5 O4 C2 124.7(13) 1_565 2_566 ?
C2 O4 Cu1 117.7(11) . . ?
O5 O4 Cu1 86.9(9) 1_565 . ?
C2 O4 Cu1 91.4(8) 2_566 . ?
C3 O5 O4 177(2) . 1_545 ?
C3 O5 C3 30.0(17) . 2_656 ?
O4 O5 C3 149.8(14) 1_545 2_656 ?
C3 O5 Cu1 122.1(14) . 1_545 ?
O4 O5 Cu1 58.0(10) 1_545 1_545 ?
C3 O5 Cu1 92.1(9) 2_656 1_545 ?
C3 O6 O1 152.3(18) . 2_666 ?
C3 O6 Cu1 125.2(14) . . ?
O1 O6 Cu1 66.4(9) 2_666 . ?
C1 C1 O2 108(2) 2_667 . ?
C1 C1 O1 123(2) 2_667 . ?
O2 C1 O1 122.9(16) . . ?
C1 C1 O2 39.6(15) 2_667 2_667 ?
O2 C1 O2 147.8(12) . 2_667 ?
O1 C1 O2 86.8(9) . 2_667 ?
C3 C3 O5 106(5) 2_656 . ?
C3 C3 O6 129(4) 2_656 . ?
O5 C3 O6 124.7(17) . . ?
C3 C3 O5 44(3) 2_656 2_656 ?
O5 C3 O5 150.0(17) . 2_656 ?
O6 C3 O5 85.2(16) . 2_656 ?
C2 C2 O4 117.0(19) 2_566 . ?
C2 C2 O3 121.4(19) 2_566 . ?
O4 C2 O3 121.6(13) . . ?
C2 C2 O4 36.7(13) 2_566 2_566 ?
O4 C2 O4 153.7(10) . 2_566 ?
O3 C2 O4 84.7(9) . 2_566 ?
C2 C2 O3 34.1(12) 2_566 2_566 ?
O4 C2 O3 82.9(9) . 2_566 ?
O3 C2 O3 155.5(10) . 2_566 ?
O4 C2 O3 70.8(8) 2_566 2_566 ?
N1 C4 N1 47.8(15) 2_557 . ?
N1 N1 C4 73(2) 2_557 2_557 ?
N1 N1 C4 59(2) 2_557 . ?
C4 N1 C4 132.2(15) 2_557 . ?

_refine_diff_density_max         1.137
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.155

_shelx_res_file                  
;
TITL DMACuF_c2_p10_s_twin in P-1
    DMACuF_c2_p11_s_mask1p5_twin1_hklf5.res
    created by SHELXL-2016/6 at 16:33:32 on 21-Mar-2018
REM P-1 (#2 in standard setting)
CELL 0.41108    5.390062 5.896905  5.720088    95.9475  88.8175  96.9576
ZERR    1.00    0.000899 0.001375  0.004414    0.0525   0.0397   0.0164
LATT  1
SFAC C H N O Cu
DISP $C -0.00006  0.00048  5.14091!source kissel
DISP $H -0.00003  0.00000  0.64127!source kissel
DISP $N  0.00062  0.00099  7.19030!source kissel
DISP $O  0.00180  0.00183 10.15475!source kissel
DISP $Cu  0.24634  0.46870 1129.00277!source kissel
UNIT 5.00 11.00 1.00 6.00 1.00
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
L.S. 50
SIZE 0.07 0.045 0.02
ACTA
BOND
FMAP 2
PLAN 20
MERG 0
WGHT    0.135600
BASF   0.60155
FVAR      27.31672
MOLE   1
CU1   5    0.500000    0.500000    0.500000    10.50000    0.02397    0.03888 =
         0.02648   -0.00810   -0.00802   -0.00507
O1    4    0.638979    0.640377    0.802317    10.50000    0.03100
O2    4    0.710523    0.581203    1.164778    10.50000    0.03266
O3    4   -0.188052    0.607456    0.354111    10.50000    0.03144
O4    4    0.219997    0.606170    0.358407    10.50000    0.03240
O5    4    0.333599   -0.186017    0.406734    10.50000    0.04121
O6    4    0.367330    0.184978    0.388148    10.50000    0.04537
C1    1    0.589483    0.536327    0.979309    10.50000    0.02164
C3    1    0.433839    0.007065    0.459690    10.50000    0.03494
C2    1    0.005209    0.547203    0.438844    10.50000    0.01624
C4    1    0.169852   -0.099594    0.937651    11.00000    0.06431
N1    3   -0.002055   -0.015630    1.088709    10.50000    0.03764
MOLE   2
HKLF 5 1 0 1 0 1 0 0 0 0 1 1 0




REM  DMACuF_c2_p10_s_twin in P-1
REM R1 =  0.0743 for     414 Fo > 4sig(Fo)  and  0.0983 for all     632 data
REM     52 parameters refined using      0 restraints

END

WGHT      0.1360      0.0000

REM Highest difference peak  1.137,  deepest hole -0.951,  1-sigma level  0.155
Q1    1   0.3482  0.5147  0.5081  11.00000  0.05    1.14
Q2    1   0.4968  0.3030  0.4831  11.00000  0.05    0.72
Q3    1  -0.2824  0.6322  0.5241  11.00000  0.05    0.71
Q4    1   0.1550 -0.0158  0.8702  11.00000  0.05    0.70
Q5    1   0.1746 -0.1931  0.9787  11.00000  0.05    0.56
Q6    1   0.1882  0.5349  0.4606  11.00000  0.05    0.50
Q7    1  -0.2030  0.4007  0.3373  11.00000  0.05    0.49
Q8    1   0.5467  0.4842  1.2759  11.00000  0.05    0.46
Q9    1   0.4020  0.0145  0.3867  11.00000  0.05    0.44
Q10   1   0.0655 -0.0191  0.5526  11.00000  0.05    0.43
Q11   1   0.0250  0.5949  0.3754  11.00000  0.05    0.41
Q12   1  -0.1520  0.7466  0.5256  11.00000  0.05    0.40
Q13   1   0.4894  0.5330  0.8700  11.00000  0.05    0.40
Q14   1   0.7721  0.7074  1.1400  11.00000  0.05    0.39
Q15   1   0.1949 -0.1809  0.4084  11.00000  0.05    0.39
Q16   1   0.3350  0.5038  0.3198  11.00000  0.05    0.39
Q17   1   0.3607 -0.0140  0.8563  11.00000  0.05    0.38
Q18   1  -0.1672  0.5185  0.3562  11.00000  0.05    0.38
Q19   1   1.0000  0.5000  1.0000  10.50000  0.05    0.37
Q20   1   0.0907  0.5150  0.1871  11.00000  0.05    0.37
;
_shelx_res_checksum              60270
