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

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

data_Mn-Formate_new_polymorph
_database_code_depnum_ccdc_archive 'CCDC 1048677'
_audit_update_record             
;
2015-02-10 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
#==============================================================================
_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
H positions were identified from fourier difference 
plots but then refined geometrically. Displacement 
parameters of H riding on C and N were constrained 
to having 1.2 and 1.5 times those on the atoms
on which they rode. 
;
_cell_length_a                   6.8568(2)
_cell_length_b                   9.3906(2)
_cell_length_c                   10.7307(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     690.94(3)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21 '
_symmetry_space_group_name_Hall  'P 2c -2n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,z
-x,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C3 H7 Mn1 N1 O6 
# Dc =      2.00 Fooo =    420.00 Mu =     18.95 M =    208.02
# Found Formula = C3 H7 Mn1 N1 O6 
# Dc =      2.00 FOOO =    420.00 Mu =     18.95 M =    208.02

_chemical_formula_sum            'C3 H7 Mn1 N1 O6'
_chemical_formula_moiety         'C3 H3 Mn O6, H4 N'
_chemical_compound_source        synthesised
_chemical_formula_weight         208.02


_cell_measurement_reflns_used    950
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.090
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    2.000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    1.895

# Sheldrick geometric approximatio 0.71 0.68 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_T_max  2.15285
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  CRYSTALS
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            9149
_reflns_number_total             1481
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections without Friedels Law is 1481 
# Number of reflections with Friedels Law is 835 
# Theoretical number of reflections is about 791 


_diffrn_reflns_theta_min         5.263
_diffrn_reflns_theta_max         27.472
_diffrn_measured_fraction_theta_max 0.994

_diffrn_reflns_theta_full        27.472
_diffrn_measured_fraction_theta_full 0.994


_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              0
_reflns_limit_h_max              8
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              -13
_reflns_limit_l_max              13

_oxford_diffrn_Wilson_B_factor   1.27
_oxford_diffrn_Wilson_scale      4.58

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

_refine_diff_density_min         -0.41
_refine_diff_density_max         0.57


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         1481
_refine_ls_number_restraints     1
_refine_ls_number_parameters     101
_oxford_refine_ls_R_factor_ref   0.0327
_refine_ls_wR_factor_ref         0.0641
_refine_ls_goodness_of_fit_ref   0.9596
_refine_ls_shift/su_max          0.0001083
_refine_ls_shift/su_mean         0.0000155


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1481
_refine_ls_R_factor_all          0.0327
_refine_ls_wR_factor_all         0.0641

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1335
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_gt          0.0617

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 0.99P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.39466(5) 0.49733(4) 0.47030(13) 0.0121 1.0000 Uani . . . . . .
O2 O 0.6509(3) 0.5981(2) 0.3920(2) 0.0187 1.0000 Uani . . . . . .
C3 C 0.7497(4) 0.7092(3) 0.4048(3) 0.0171 1.0000 Uani . . . . . .
O4 O 0.7311(3) 0.80214(19) 0.4877(2) 0.0193 1.0000 Uani . . . . . .
O5 O 0.5102(3) 0.5361(2) 0.6571(2) 0.0199 1.0000 Uani . . . . . .
C6 C 0.6840(4) 0.5317(3) 0.6858(3) 0.0169 1.0000 Uani . . . . . .
O7 O 0.7530(3) 0.5431(2) 0.7937(2) 0.0197 1.0000 Uani . . . . . .
O8 O 0.1492(3) 0.4017(2) 0.5681(2) 0.0188 1.0000 Uani . . . . . .
C9 C 0.0517(4) 0.2900(3) 0.5543(3) 0.0169 1.0000 Uani . . . . . .
O10 O 0.0627(3) 0.20356(17) 0.4651(2) 0.0169 1.0000 Uani . . . . . .
N11 N -0.1486(3) 0.3720(3) 0.2611(2) 0.0175 1.0000 Uani . . . . . .
H31 H 0.8511 0.7251 0.3449 0.0201 1.0000 Uiso R . . . . .
H61 H 0.7767 0.5186 0.6182 0.0211 1.0000 Uiso R . . . . .
H91 H -0.0399 0.2671 0.6192 0.0203 1.0000 Uiso R . . . . .
H114 H -0.2313 0.4460 0.2686 0.0280 1.0000 Uiso R . . . . .
H113 H -0.1545 0.3381 0.1839 0.0272 1.0000 Uiso R . . . . .
H112 H -0.1847 0.3038 0.3154 0.0276 1.0000 Uiso R . . . . .
H111 H -0.0273 0.4016 0.2778 0.0279 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.01221(19) 0.01105(19) 0.0130(2) -0.00060(14) -0.0003(2) 0.00033(13)
O2 0.0182(10) 0.0171(10) 0.0206(11) -0.0025(8) 0.0028(8) -0.0042(8)
C3 0.0169(13) 0.0171(13) 0.0172(14) 0.0001(11) 0.0022(11) -0.0022(11)
O4 0.0225(10) 0.0139(8) 0.0215(12) -0.0027(8) 0.0015(9) -0.0030(7)
O5 0.0150(9) 0.0273(11) 0.0173(10) -0.0015(9) -0.0014(8) 0.0008(8)
C6 0.0159(13) 0.0161(13) 0.0188(15) 0.0001(11) -0.0019(11) 0.0000(11)
O7 0.0177(10) 0.0271(11) 0.0142(10) 0.0010(9) -0.0022(8) -0.0022(8)
O8 0.0199(11) 0.0145(10) 0.0221(12) -0.0038(8) 0.0026(8) -0.0032(8)
C9 0.0161(13) 0.0152(13) 0.0194(15) 0.0013(11) 0.0007(11) -0.0014(10)
O10 0.0188(8) 0.0124(8) 0.0195(10) -0.0013(10) 0.0002(10) -0.0022(6)
N11 0.0175(11) 0.0174(11) 0.0176(13) 0.0022(10) -0.0015(10) 0.0000(9)

_refine_ls_extinction_coef       62(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.4367(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O10 3_555 2.2113(17) yes
Mn1 . O4 3_465 2.1995(18) yes
Mn1 . O7 4_664 2.181(2) yes
Mn1 . O2 . 2.165(2) yes
Mn1 . O5 . 2.186(2) yes
Mn1 . O8 . 2.177(2) yes
O2 . C3 . 1.252(4) yes
C3 . O4 . 1.252(3) yes
C3 . H31 . 0.959 no
O5 . C6 . 1.231(4) yes
C6 . O7 . 1.255(4) yes
C6 . H61 . 0.973 no
O8 . C9 . 1.253(3) yes
C9 . O10 . 1.257(4) yes
C9 . H91 . 0.962 no
N11 . H114 . 0.901 no
N11 . H113 . 0.888 no
N11 . H112 . 0.900 no
N11 . H111 . 0.896 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O10 3_555 Mn1 . O4 3_465 176.51(11) yes
O10 3_555 Mn1 . O7 4_664 94.12(9) yes
O4 3_465 Mn1 . O7 4_664 89.19(8) yes
O10 3_555 Mn1 . O2 . 86.58(8) yes
O4 3_465 Mn1 . O2 . 94.15(8) yes
O7 4_664 Mn1 . O2 . 96.63(8) yes
O10 3_555 Mn1 . O5 . 88.63(9) yes
O4 3_465 Mn1 . O5 . 87.97(9) yes
O7 4_664 Mn1 . O5 . 173.54(8) yes
O2 . Mn1 . O5 . 89.36(8) yes
O10 3_555 Mn1 . O8 . 93.61(8) yes
O4 3_465 Mn1 . O8 . 85.31(7) yes
O7 4_664 Mn1 . O8 . 89.34(8) yes
O2 . Mn1 . O8 . 174.00(10) yes
O5 . Mn1 . O8 . 84.65(8) yes
Mn1 . O2 . C3 . 139.53(19) yes
O2 . C3 . O4 . 127.2(3) yes
O2 . C3 . H31 . 116.6 no
O4 . C3 . H31 . 116.2 no
Mn1 3_565 O4 . C3 . 118.99(19) yes
Mn1 . O5 . C6 . 125.1(2) yes
O5 . C6 . O7 . 126.4(3) yes
O5 . C6 . H61 . 116.7 no
O7 . C6 . H61 . 116.9 no
Mn1 4_665 O7 . C6 . 127.69(19) yes
Mn1 . O8 . C9 . 134.50(19) yes
O8 . C9 . O10 . 126.8(3) yes
O8 . C9 . H91 . 116.8 no
O10 . C9 . H91 . 116.4 no
Mn1 3_455 O10 . C9 . 120.04(19) yes
H114 . N11 . H113 . 109.3 no
H114 . N11 . H112 . 108.6 no
H113 . N11 . H112 . 109.7 no
H114 . N11 . H111 . 109.0 no
H113 . N11 . H111 . 109.9 no
H112 . N11 . H111 . 110.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N11 . H114 . O2 1_455 145.09(9) 0.901 2.109 2.893(4) yes
N11 . H114 . O5 4_564 122.82(8) 0.901 2.262 2.853(4) yes
N11 . H113 . O4 2_544 163.78(8) 0.888 2.196 3.059(4) yes
N11 . H112 . O7 2_544 133.35(7) 0.900 2.504 3.190(4) yes
N11 . H112 . O10 3_455 131.46(7) 0.900 2.364 3.036(4) yes
N11 . H111 . O7 4_664 172.79(9) 0.896 1.959 2.850(4) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 09/12/13 at 10:22:00
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
REM TOO MANY H ATOMS ON N   (  11), - 4 
RIDE N   (  11,X'S) H   ( 114,X'S) H   ( 113,X'S) H   ( 112,X'S) H   ( 111,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 09/12/13 at 10:22:00
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Mn-Formate
_database_code_depnum_ccdc_archive 'CCDC 1048678'
_audit_update_record             
;
2015-02-10 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2015-02-06
_audit_creation_method           CRYSTALS_ver_14.61

_oxford_structure_analysis_title 002jmml13
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   12.65088(13)
_cell_length_b                   12.65088(13)
_cell_length_c                   8.54951(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1184.987(12)

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63 '
_symmetry_space_group_name_Hall  'P 6c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x-y,x,z+1/2
-y,x-y,z
-x,-y,z+1/2
-x+y,-x,z
y,-x+y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0070 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3290 0.6900 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            6

# Given Formula = C3 H7 Mn1 N1 O6 
# Dc =      1.75 Fooo =    630.00 Mu =     16.57 M =    208.02
# Found Formula = C3 H7 Mn1 N1 O6 
# Dc =      1.75 FOOO =    630.00 Mu =     16.57 M =    208.02

_chemical_formula_sum            'C3 H7 Mn1 N1 O6'
_chemical_formula_moiety         'C3 H7 Mn1 N1 O6'
_chemical_compound_source        .
_chemical_formula_weight         208.02


_cell_measurement_reflns_used    7771
_cell_measurement_theta_min      3
_cell_measurement_theta_max      32
_cell_measurement_temperature    30

_exptl_crystal_description       plate
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.005
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_max          0.010

_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             630.000
_exptl_absorpt_coefficient_mu    1.657

# Sheldrick geometric approximatio 0.98 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  1.00
_diffrn_source                   Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_monochromator  Synchrotron
_diffrn_detector                 CCD
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_method       'profile data from ω-scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Refinement of known structure'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      30
_diffrn_reflns_number            26983
_reflns_number_total             2878
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 2878 
# Number of reflections with Friedels Law is 1545 
# Theoretical number of reflections is about 1479 


_diffrn_reflns_theta_min         1.802
_diffrn_reflns_theta_max         31.782
_diffrn_measured_fraction_theta_max 0.982

_diffrn_reflns_theta_full        30.510
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              -16
_reflns_limit_h_max              0
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              -12
_reflns_limit_l_max              13

_oxford_diffrn_Wilson_B_factor   0.48
_oxford_diffrn_Wilson_scale      0.04

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

_refine_diff_density_min         -0.65
_refine_diff_density_max         0.67


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     55
_refine_ls_number_parameters     131
_oxford_refine_ls_R_factor_ref   0.0388
_refine_ls_wR_factor_ref         0.0744
_refine_ls_goodness_of_fit_ref   0.9457
_refine_ls_shift/su_max          0.0059250
_refine_ls_shift/su_mean         0.0004463


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2863
_refine_ls_R_factor_all          0.0388
_refine_ls_wR_factor_all         0.0744

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2736
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_gt          0.0702

_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_abs_structure_details 'Flack (1983), 1333 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.166E+04 0.266E+04 0.165E+04 689. 169. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.6204(2) 0.8125(2) 0.6556(3) 0.0153 1.0000 Uani D . . . . .
C2 C 0.51526(19) 0.46776(19) 0.6535(3) 0.0111 1.0000 Uani D . . . . .
C3 C 0.84836(18) 0.71366(18) 0.6940(3) 0.0057 1.0000 Uani D . . . . .
Mn1 Mn 0.66943(2) 0.66398(2) 0.41885(16) 0.0048 1.0000 Uani . . . . . .
O1 O 0.56676(14) 0.72614(14) 0.5625(2) 0.0098 1.0000 Uani D . . . . .
O2 O 0.57205(15) 0.83451(14) 0.7706(2) 0.0088 1.0000 Uani D . . . . .
O3 O 0.60161(14) 0.49972(14) 0.5614(2) 0.0087 1.0000 Uani D . . . . .
O4 O 0.49091(13) 0.39816(14) 0.7689(2) 0.0087 1.0000 Uani D . . . . .
O5 O 0.82729(14) 0.75692(14) 0.5735(2) 0.0087 1.0000 Uani D . . . . .
O6 O 0.94017(14) 0.77094(14) 0.7812(2) 0.0086 1.0000 Uani D . . . . .
N1 N 0.3333 0.6667 0.3669(4) 0.0113 1.0000 Uani DS T . . . .
N2 N 0.6667 0.3333 0.3699(4) 0.0099 1.0000 Uani DS T . . . .
N3 N 1.0000 1.0000 0.9762(4) 0.0082 1.0000 Uani DS T . . . .
H1 H 0.7038(16) 0.8671(15) 0.637(2) 0.017(2) 1.0000 Uiso D . . . . .
H2 H 0.4618(15) 0.4984(13) 0.634(2) 0.014(2) 1.0000 Uiso D . . . . .
H3 H 0.7928(15) 0.6332(16) 0.720(2) 0.012(2) 1.0000 Uiso D . . . . .
H11 H 0.2640(16) 0.6598(19) 0.3289(19) 0.019(2) 1.0000 Uiso D . . . . .
H12 H 0.3333 0.6667 0.474(2) 0.015(2) 1.0000 Uiso DS . . . . .
H21 H 0.709(3) 0.299(3) 0.3358(16) 0.018(2) 1.0000 Uiso D . . . . .
H22 H 0.6667 0.3333 0.474(2) 0.015(2) 1.0000 Uiso DS . . . . .
H31 H 1.0415(18) 1.0767(16) 1.0128(19) 0.017(2) 1.0000 Uiso D . . . . .
H32 H 1.0000 1.0000 0.872(2) 0.018(2) 1.0000 Uiso DS . . . . .
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
C1 0.0091(9) 0.0160(10) 0.0198(11) -0.0121(8) -0.0005(8) 0.0056(8)
C2 0.0069(8) 0.0087(8) 0.0168(10) 0.0056(7) 0.0017(7) 0.0034(7)
C3 0.0065(7) 0.0075(8) 0.0019(7) 0.0010(6) 0.0016(6) 0.0027(6)
Mn1 0.00646(11) 0.00595(11) 0.00391(10) -0.00092(12) 0.00068(12) 0.00444(8)
O1 0.0112(6) 0.0076(6) 0.0103(6) -0.0042(5) 0.0011(5) 0.0044(5)
O2 0.0131(7) 0.0077(6) 0.0067(6) -0.0024(5) 0.0004(5) 0.0059(5)
O3 0.0113(6) 0.0079(6) 0.0058(6) -0.0007(5) 0.0000(5) 0.0039(5)
O4 0.0080(6) 0.0128(7) 0.0064(6) 0.0019(5) 0.0004(5) 0.0060(5)
O5 0.0097(6) 0.0072(6) 0.0080(7) 0.0018(5) -0.0010(5) 0.0033(5)
O6 0.0076(6) 0.0073(6) 0.0093(7) -0.0028(5) -0.0036(5) 0.0026(5)
N1 0.0113(8) 0.0113(8) 0.0114(13) 0.0000 0.0000 0.0056(4)
N2 0.0101(8) 0.0101(8) 0.0095(12) 0.0000 0.0000 0.0050(4)
N3 0.0083(7) 0.0083(7) 0.0079(12) 0.0000 0.0000 0.0042(3)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.98(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . O1 . 1.244(3) yes
C1 . O2 . 1.260(3) yes
C1 . H1 . 0.941(18) no
C2 . O3 . 1.239(3) yes
C2 . O4 . 1.254(3) yes
C2 . H2 . 0.947(18) no
C3 . O5 . 1.256(2) yes
C3 . O6 . 1.260(2) yes
C3 . H3 . 0.930(18) no
Mn1 . O4 4_664 2.1865(15) yes
Mn1 . O6 6_564 2.1856(16) yes
Mn1 . O2 2_654 2.1688(15) yes
Mn1 . O1 . 2.1989(16) yes
Mn1 . O3 . 2.1808(15) yes
Mn1 . O5 . 2.1844(16) yes
N1 . H11 3_665 0.898(18) no
N1 . H11 5_565 0.898(18) no
N1 . H11 . 0.898(18) no
N1 . H12 . 0.912 no
N2 . H21 5_665 0.892(18) no
N2 . H21 3_655 0.892(18) no
N2 . H21 . 0.892(18) no
N2 . H22 . 0.890 no
N3 . H31 5_675 0.898(17) no
N3 . H31 3_765 0.898(17) no
N3 . H31 . 0.898(17) no
N3 . H32 . 0.889 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . C1 . O2 . 125.5(2) yes
O1 . C1 . H1 . 117.1(12) no
O2 . C1 . H1 . 117.4(12) no
O3 . C2 . O4 . 126.6(2) yes
O3 . C2 . H2 . 116.6(12) no
O4 . C2 . H2 . 116.8(12) no
O5 . C3 . O6 . 124.75(19) yes
O5 . C3 . H3 . 117.6(12) no
O6 . C3 . H3 . 117.6(12) no
O4 4_664 Mn1 . O6 6_564 91.32(6) yes
O4 4_664 Mn1 . O2 2_654 90.60(6) yes
O6 6_564 Mn1 . O2 2_654 90.22(6) yes
O4 4_664 Mn1 . O1 . 81.27(6) yes
O6 6_564 Mn1 . O1 . 97.04(6) yes
O2 2_654 Mn1 . O1 . 169.20(6) yes
O4 4_664 Mn1 . O3 . 97.62(6) yes
O6 6_564 Mn1 . O3 . 169.14(6) yes
O2 2_654 Mn1 . O3 . 83.57(6) yes
O1 . Mn1 . O3 . 90.42(6) yes
O4 4_664 Mn1 . O5 . 169.28(6) yes
O6 6_564 Mn1 . O5 . 82.45(6) yes
O2 2_654 Mn1 . O5 . 98.11(6) yes
O1 . Mn1 . O5 . 90.80(6) yes
O3 . Mn1 . O5 . 89.59(6) yes
Mn1 . O1 . C1 . 120.76(15) yes
Mn1 6_565 O2 . C1 . 124.68(15) yes
Mn1 . O3 . C2 . 121.92(14) yes
Mn1 4_665 O4 . C2 . 124.87(14) yes
Mn1 . O5 . C3 . 126.73(13) yes
Mn1 2_655 O6 . C3 . 119.41(13) yes
H11 3_665 N1 . H11 5_565 107.6(11) no
H11 3_665 N1 . H11 . 107.6(11) no
H11 5_565 N1 . H11 . 107.6(11) no
H11 3_665 N1 . H12 . 111.2 no
H11 5_565 N1 . H12 . 111.2 no
H11 . N1 . H12 . 111.2 no
H21 5_665 N2 . H21 3_655 109.9(8) no
H21 5_665 N2 . H21 . 109.9(8) no
H21 3_655 N2 . H21 . 109.9(8) no
H21 5_665 N2 . H22 . 109.1 no
H21 3_655 N2 . H22 . 109.1 no
H21 . N2 . H22 . 109.1 no
H31 5_675 N3 . H31 3_765 108.6(11) no
H31 5_675 N3 . H31 . 108.6(11) no
H31 3_765 N3 . H31 . 108.6(11) no
H31 5_675 N3 . H32 . 110.4 no
H31 3_765 N3 . H32 . 110.4 no
H31 . N3 . H32 . 110.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C1 . H1 . O6 5_675 125.1(15) 0.941 2.475 3.114(4) yes
C2 . H2 . O2 5_565 124.8(15) 0.947 2.505 3.142(4) yes
C3 . H3 . O3 . 123.2(15) 0.930 2.540 3.147(4) yes
N1 . H11 . O4 2_554 127.9(17) 0.898 2.212 2.853(4) yes
N2 . H21 . O2 6_554 166(3) 0.892 1.942 2.817(4) yes
N3 . H31 . O5 4_775 164.2(19) 0.898 1.990 2.864(4) yes
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co-Formate
_database_code_depnum_ccdc_archive 'CCDC 1048679'
_audit_update_record             
;
2015-02-10 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
#==============================================================================
_audit_creation_date             2015-02-06
_audit_creation_method           CRYSTALS_ver_14.61

_oxford_structure_analysis_title 002jmml13
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   12.5965(2)
_cell_length_b                   12.5965(1)
_cell_length_c                   8.2395(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1132.221(14)

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63 '
_symmetry_space_group_name_Hall  P6c
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x-y,x,z+1/2
-y,x-y,z
-x,-y,z+1/2
-x+y,-x,z
y,-x+y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0070 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.2980 0.9220 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            6

# Given Formula = C0.17 H0.17 Co0.17 N0.17 O0.17 
# Dc =      0.15 Fooo =    642.00 Mu =      3.60 M =     16.99
# Found Formula = C3 H7 Co1 N1 O6 
# Dc =      1.87 FOOO =    642.00 Mu =     22.59 M =    212.02

_chemical_formula_sum            'C3 H7 Co1 N1 O6'
_chemical_formula_moiety         'C3 H7 Co1 N1 O6'
_chemical_compound_source        .
_chemical_formula_weight         212.02


_cell_measurement_reflns_used    5120
_cell_measurement_theta_min      3
_cell_measurement_theta_max      31
_cell_measurement_temperature    30

_exptl_crystal_description       plate
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.005
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_max          0.010

_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             642.000
_exptl_absorpt_coefficient_mu    2.259

# Sheldrick geometric approximatio 0.98 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  1.00
_diffrn_source                   Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_monochromator  Synchrotron
_diffrn_detector                 CCD
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_radiation_wavelength     0.68890
_diffrn_measurement_method       'profile data from ω-scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Refinement of known structure'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      30
_diffrn_reflns_number            25583
_reflns_number_total             2729
_diffrn_reflns_av_R_equivalents  0.058
# Number of reflections without Friedels Law is 2729 
# Number of reflections with Friedels Law is 1471 
# Theoretical number of reflections is about 1404 


_diffrn_reflns_theta_min         1.809
_diffrn_reflns_theta_max         31.703
_diffrn_measured_fraction_theta_max 0.985

_diffrn_reflns_theta_full        30.435
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -15
_reflns_limit_h_max              0
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              -12
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -0.74
_refine_diff_density_max         0.65


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         2712
_refine_ls_number_restraints     55
_refine_ls_number_parameters     131
_oxford_refine_ls_R_factor_ref   0.0430
_refine_ls_wR_factor_ref         0.0734
_refine_ls_goodness_of_fit_ref   0.9563
_refine_ls_shift/su_max          0.0041757
_refine_ls_shift/su_mean         0.0002522


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2714
_refine_ls_R_factor_all          0.0432
_refine_ls_wR_factor_all         0.0737

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2231
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_gt          0.0594

_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_abs_structure_details 'Flack (1983), 1258 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.173E+04 0.277E+04 0.162E+04 646. 104. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.6266(2) 0.8119(2) 0.6640(3) 0.0113 1.0000 Uani D . . . . .
C2 C 0.5138(2) 0.4737(2) 0.6572(3) 0.0081 1.0000 Uani D . . . . .
C3 C 0.8488(2) 0.7068(2) 0.6853(3) 0.0067 1.0000 Uani D . . . . .
Co1 Co 0.66864(2) 0.66474(2) 0.41874(18) 0.0041 1.0000 Uani . . . . . .
O1 O 0.57332(16) 0.72776(16) 0.5626(3) 0.0080 1.0000 Uani D . . . . .
O2 O 0.57500(16) 0.83808(16) 0.7747(3) 0.0080 1.0000 Uani D . . . . .
O3 O 0.60166(16) 0.50513(15) 0.5610(3) 0.0082 1.0000 Uani D . . . . .
O4 O 0.48895(15) 0.39981(16) 0.7735(2) 0.0074 1.0000 Uani D . . . . .
O5 O 0.82542(16) 0.75467(16) 0.5659(2) 0.0074 1.0000 Uani D . . . . .
O6 O 0.93935(16) 0.76388(16) 0.7785(2) 0.0078 1.0000 Uani D . . . . .
N1 N 0.3333 0.6667 0.3711(5) 0.0114 1.0000 Uani DS T . . . .
N2 N 0.6667 0.3333 0.3728(5) 0.0096 1.0000 Uani DS T . . . .
N3 N 1.0000 1.0000 0.9665(6) 0.0076 1.0000 Uani DS T . . . .
H1 H 0.7126(16) 0.8611(15) 0.656(2) 0.0175(19) 1.0000 Uiso D . . . . .
H2 H 0.4608(15) 0.5048(13) 0.641(2) 0.0133(19) 1.0000 Uiso D . . . . .
H3 H 0.7955(15) 0.6236(16) 0.708(2) 0.0105(19) 1.0000 Uiso D . . . . .
H11 H 0.390(3) 0.648(4) 0.3336(16) 0.0161(19) 1.0000 Uiso D . . . . .
H12 H 0.3333 0.6667 0.480(2) 0.016(2) 1.0000 Uiso DS . . . . .
H21 H 0.5922(19) 0.277(3) 0.3356(16) 0.0163(19) 1.0000 Uiso D . . . . .
H22 H 0.6667 0.3333 0.481(2) 0.016(2) 1.0000 Uiso DS . . . . .
H31 H 0.9236(17) 0.977(4) 1.0036(16) 0.0160(19) 1.0000 Uiso D . . . . .
H32 H 1.0000 1.0000 0.857(2) 0.017(2) 1.0000 Uiso DS . . . . .
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
C1 0.0069(9) 0.0099(10) 0.0174(13) -0.0075(8) -0.0011(8) 0.0044(8)
C2 0.0049(8) 0.0072(9) 0.0117(12) 0.0001(7) -0.0027(7) 0.0027(7)
C3 0.0074(9) 0.0071(9) 0.0047(11) 0.0018(7) 0.0016(7) 0.0028(7)
Co1 0.00444(11) 0.00481(11) 0.00386(10) -0.00028(14) 0.00018(14) 0.00303(9)
O1 0.0078(7) 0.0083(7) 0.0082(7) -0.0006(6) -0.0003(6) 0.0042(6)
O2 0.0105(7) 0.0068(7) 0.0073(7) -0.0003(6) 0.0016(6) 0.0048(6)
O3 0.0093(7) 0.0067(7) 0.0078(7) -0.0001(6) -0.0002(6) 0.0034(6)
O4 0.0075(7) 0.0100(7) 0.0062(7) 0.0020(6) 0.0008(6) 0.0054(6)
O5 0.0082(7) 0.0070(7) 0.0074(7) 0.0010(6) -0.0012(6) 0.0041(6)
O6 0.0074(7) 0.0075(7) 0.0070(7) -0.0011(6) -0.0026(6) 0.0026(6)
N1 0.0090(9) 0.0090(9) 0.0162(17) 0.0000 0.0000 0.0045(4)
N2 0.0096(9) 0.0096(9) 0.0098(15) 0.0000 0.0000 0.0048(4)
N3 0.0088(8) 0.0088(8) 0.0054(15) 0.0000 0.0000 0.0044(4)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.96(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . O1 . 1.248(3) yes
C1 . O2 . 1.257(3) yes
C1 . H1 . 0.944(18) no
C2 . O3 . 1.254(3) yes
C2 . O4 . 1.261(3) yes
C2 . H2 . 0.937(18) no
C3 . O5 . 1.264(3) yes
C3 . O6 . 1.259(3) yes
C3 . H3 . 0.937(17) no
Co1 . O4 4_664 2.1025(17) yes
Co1 . O6 6_564 2.1005(17) yes
Co1 . O2 2_654 2.0971(18) yes
Co1 . O1 . 2.1050(18) yes
Co1 . O3 . 2.1054(18) yes
Co1 . O5 . 2.1017(18) yes
N1 . H11 5_565 0.915(17) no
N1 . H11 3_665 0.915(17) no
N1 . H11 . 0.915(17) no
N1 . H12 . 0.895 no
N2 . H21 5_665 0.902(17) no
N2 . H21 3_655 0.902(17) no
N2 . H21 . 0.902(17) no
N2 . H22 . 0.894 no
N3 . H31 3_765 0.908(17) no
N3 . H31 5_675 0.908(17) no
N3 . H31 . 0.908(17) no
N3 . H32 . 0.899 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . C1 . O2 . 125.4(2) yes
O1 . C1 . H1 . 117.8(12) no
O2 . C1 . H1 . 116.8(12) no
O3 . C2 . O4 . 124.6(2) yes
O3 . C2 . H2 . 118.6(12) no
O4 . C2 . H2 . 116.8(12) no
O5 . C3 . O6 . 124.2(2) yes
O5 . C3 . H3 . 118.6(12) no
O6 . C3 . H3 . 117.2(12) no
O4 4_664 Co1 . O6 6_564 91.93(7) yes
O4 4_664 Co1 . O2 2_654 91.82(7) yes
O6 6_564 Co1 . O2 2_654 90.77(7) yes
O4 4_664 Co1 . O1 . 81.96(6) yes
O6 6_564 Co1 . O1 . 96.24(6) yes
O2 2_654 Co1 . O1 . 170.76(7) yes
O4 4_664 Co1 . O3 . 95.61(7) yes
O6 6_564 Co1 . O3 . 170.32(7) yes
O2 2_654 Co1 . O3 . 82.94(6) yes
O1 . Co1 . O3 . 90.84(7) yes
O4 4_664 Co1 . O5 . 171.12(7) yes
O6 6_564 Co1 . O5 . 82.45(6) yes
O2 2_654 Co1 . O5 . 95.11(6) yes
O1 . Co1 . O5 . 91.78(7) yes
O3 . Co1 . O5 . 90.76(7) yes
Co1 . O1 . C1 . 122.05(16) yes
Co1 6_565 O2 . C1 . 123.81(16) yes
Co1 . O3 . C2 . 121.53(16) yes
Co1 4_665 O4 . C2 . 123.77(15) yes
Co1 . O5 . C3 . 124.93(15) yes
Co1 2_655 O6 . C3 . 120.49(15) yes
H11 5_565 N1 . H11 3_665 109.2(8) no
H11 5_565 N1 . H11 . 109.2(8) no
H11 3_665 N1 . H11 . 109.2(8) no
H11 5_565 N1 . H12 . 109.7 no
H11 3_665 N1 . H12 . 109.7 no
H11 . N1 . H12 . 109.7 no
H21 5_665 N2 . H21 3_655 109.1(8) no
H21 5_665 N2 . H21 . 109.1(8) no
H21 3_655 N2 . H21 . 109.1(8) no
H21 5_665 N2 . H22 . 109.9 no
H21 3_655 N2 . H22 . 109.9 no
H21 . N2 . H22 . 109.9 no
H31 3_765 N3 . H31 5_675 109.3(8) no
H31 3_765 N3 . H31 . 109.3(8) no
H31 5_675 N3 . H31 . 109.3(8) no
H31 3_765 N3 . H32 . 109.7 no
H31 5_675 N3 . H32 . 109.7 no
H31 . N3 . H32 . 109.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C1 . H1 . O6 5_675 122.7(15) 0.944 2.403 3.019(4) yes
C2 . H2 . O2 5_565 123.9(15) 0.937 2.434 3.058(4) yes
C3 . H3 . O3 . 121.5(15) 0.937 2.451 3.047(4) yes
N1 . H11 . O4 4_664 174.4(19) 0.915 1.957 2.870(4) yes
N2 . H21 . O2 4_664 174(3) 0.902 1.932 2.830(4) yes
N3 . H31 . O5 6_565 175.4(14) 0.908 1.968 2.874(4) yes


#==============================================================================
# start Validation Reply Form
#==============================================================================
_vrf_PLAT113_I                   
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space group.      P6322 Check 
RESPONSE: The symmetry has been checked and is broken by the hydrogen atoms
as shown by the neutron data.
;
#==============================================================================
# end Validation Reply Form
#==============================================================================
