# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_SOLVE_4K_a
_database_code_depnum_ccdc_archive 'CCDC 2288634'
loop_
_audit_author_name
_audit_author_address
'Siya T. Hulushe'
;Rhodes University
South Africa
;
_audit_update_record             
;
2024-03-11 deposited with the CCDC.	2024-04-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2016/6
_chemical_name_systematic        ?
_chemical_name_common            'dicobalt(II) pyromellitate dodecahydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H9 Co O8, 2(H2 O)'
_chemical_formula_sum            'C5 H13 Co O10'
_chemical_formula_weight         292.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   10.7969(8)
_cell_length_b                   11.1079(8)
_cell_length_c                   11.4544(8)
_cell_angle_alpha                82.796(3)
_cell_angle_beta                 62.783(2)
_cell_angle_gamma                62.288(3)
_cell_volume                     1074.84(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      2.732
_cell_measurement_theta_max      26.43
_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_F_000             600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.093
_exptl_absorpt_coefficient_mu    1.638
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6435
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 TWINABS (v.2012/1): Sheldrick G.M. Georg-August-Universitat, 
 Gottingen, Gottingen, Germany, 2012. 
;
_diffrn_radiation_probe          x-ray
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-IV CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.12
_diffrn_reflns_number            53246
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.012
_diffrn_reflns_theta_max         26.454
_diffrn_reflns_theta_full        25.125
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4428
_reflns_number_gt                3025
_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       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Carbon-bound H atoms were placed in calculated positions and were included in
the refinement in the riding model approximation, with Uiso(H) set to
1.2 Ueq(C).

The H atoms of the water molecules were located on a difference Fourier map and
refined with the O---H bond lengths and the H---O---H bond angles restrained to
0.85 Å and 109 ° respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0526P)²+1.6438P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4428
_refine_ls_number_parameters     399
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1207
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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
Co1 Co 0.500000 1.000000 0.500000 0.01539(17) Uani 1 2 d S . P . .
Co2 Co 1.000000 0.500000 1.000000 0.01568(18) Uani 1 2 d S . P . .
Co3 Co 0.500000 0.500000 1.000000 0.01603(18) Uani 1 2 d S . P . .
Co4 Co 0.000000 1.000000 0.500000 0.01499(17) Uani 1 2 d S . P . .
O8 O 0.2114(3) 0.8268(2) 0.4654(2) 0.0183(5) Uani 1 1 d . . . . .
O1 O 0.7178(3) 0.8274(2) 0.4580(2) 0.0179(5) Uani 1 1 d . . . . .
O5 O 0.4552(3) 0.4977(2) 0.8383(2) 0.0176(5) Uani 1 1 d . . . . .
O4 O 0.9620(3) 0.5068(2) 0.8342(2) 0.0184(5) Uani 1 1 d . . . . .
O3 O 1.0181(3) 0.6746(3) 0.7379(2) 0.0227(6) Uani 1 1 d . . . . .
O12 O 0.7553(3) 0.5969(3) 1.1314(3) 0.0220(6) Uani 1 1 d . . . . .
O15 O -0.1067(4) 0.9355(3) 0.6828(3) 0.0218(6) Uani 1 1 d . . . . .
O16 O 0.0472(4) 1.1061(3) 0.5981(3) 0.0205(6) Uani 1 1 d . . . . .
O11 O 0.9891(4) 0.3205(3) 1.0288(3) 0.0292(7) Uani 1 1 d . . . . .
O6 O 0.4913(3) 0.6772(3) 0.7516(2) 0.0246(6) Uani 1 1 d . . . . .
O2 O 0.7115(3) 0.6623(2) 0.3709(2) 0.0196(5) Uani 1 1 d . . . . .
O14 O 0.4358(4) 0.7093(3) 0.9942(3) 0.0237(6) Uani 1 1 d . . . . .
O10 O 0.4175(4) 0.9339(3) 0.6859(3) 0.0236(6) Uani 1 1 d . . . . .
O9 O 0.4461(4) 0.8868(3) 0.4184(3) 0.0219(6) Uani 1 1 d . . . . .
O3W O -0.3979(4) 0.9536(4) 0.8005(3) 0.0286(7) Uani 1 1 d . . . . .
O1W O 0.1285(4) 1.0726(3) 0.8855(3) 0.0289(7) Uani 1 1 d . . . . .
O7 O 0.2126(3) 0.6649(2) 0.3671(2) 0.0200(6) Uani 1 1 d . . . . .
O2W O -0.1318(4) 1.0714(4) 0.8990(3) 0.0314(7) Uani 1 1 d . . . . .
O4W O 0.6018(4) 0.8163(4) 1.0201(3) 0.0310(7) Uani 1 1 d . . . . .
O13 O 0.7292(3) 0.4445(3) 0.8642(3) 0.0297(7) Uani 1 1 d . . . . .
C7 C 0.4959(4) 0.5301(3) 0.6168(3) 0.0149(7) Uani 1 1 d . . . . .
C4 C 1.0030(4) 0.5328(4) 0.6124(3) 0.0164(7) Uani 1 1 d . . . . .
C8 C 0.3904(4) 0.6238(4) 0.5740(3) 0.0170(7) Uani 1 1 d . . . . .
C3 C 0.8966(4) 0.6276(4) 0.5699(3) 0.0168(7) Uani 1 1 d . . . . .
C1 C 0.7661(4) 0.7026(3) 0.4245(3) 0.0153(7) Uani 1 1 d . . . . .
C2 C 0.8922(4) 0.5977(3) 0.4579(3) 0.0150(7) Uani 1 1 d . . . . .
C5 C 0.9956(4) 0.5740(3) 0.7372(3) 0.0157(7) Uani 1 1 d . . . . .
C6 C 0.4815(4) 0.5707(4) 0.7450(3) 0.0165(7) Uani 1 1 d . . . . .
C10 C 0.2638(4) 0.7023(4) 0.4257(3) 0.0164(7) Uani 1 1 d . . . . .
C9 C 0.3912(4) 0.5969(3) 0.4583(3) 0.0160(7) Uani 1 1 d . . . . .
H13A H 0.795(5) 0.465(4) 0.860(4) 0.024(12) Uiso 1 1 d . . . . .
H1WB H 0.040(6) 1.075(5) 0.880(4) 0.041(14) Uiso 1 1 d . . . . .
H14A H 0.494(7) 0.737(6) 0.997(5) 0.063(19) Uiso 1 1 d . . . . .
H11B H 1.038(6) 0.261(5) 0.987(5) 0.038(17) Uiso 1 1 d . . . . .
H12B H 0.694(5) 0.559(5) 1.144(4) 0.035(13) Uiso 1 1 d . . . . .
H9B H 0.362(6) 0.878(4) 0.437(4) 0.031(12) Uiso 1 1 d . . . . .
H15A H -0.202(5) 0.957(4) 0.710(4) 0.026(12) Uiso 1 1 d . . . . .
H16B H 0.127(6) 1.120(5) 0.572(4) 0.033(13) Uiso 1 1 d . . . . .
H3 H 0.823(5) 0.715(5) 0.621(4) 0.035(12) Uiso 1 1 d . . . . .
H15B H -0.060(5) 0.856(5) 0.683(4) 0.027(13) Uiso 1 1 d . . . . .
H10B H 0.325(7) 0.979(6) 0.744(6) 0.065(19) Uiso 1 1 d . . . . .
H1WA H 0.131(5) 1.035(4) 0.939(4) 0.020(13) Uiso 1 1 d . . . . .
H10A H 0.438(5) 0.855(5) 0.689(4) 0.028(13) Uiso 1 1 d . . . . .
H9A H 0.523(7) 0.807(6) 0.399(6) 0.068(19) Uiso 1 1 d . . . . .
H11A H 0.994(5) 0.297(5) 1.098(5) 0.039(14) Uiso 1 1 d . . . . .
H16A H -0.031(6) 1.184(5) 0.617(5) 0.041(14) Uiso 1 1 d . . . . .
H2WB H -0.110(5) 1.039(5) 0.837(5) 0.029(14) Uiso 1 1 d . . . . .
H2WA H -0.209(7) 1.140(6) 0.912(5) 0.058(19) Uiso 1 1 d . . . . .
H4WB H 0.664(8) 0.758(7) 1.038(6) 0.07(2) Uiso 1 1 d . . . . .
H3WA H -0.384(6) 0.898(5) 0.839(5) 0.032(15) Uiso 1 1 d . . . . .
H14B H 0.451(6) 0.720(5) 0.920(5) 0.043(15) Uiso 1 1 d . . . . .
H13B H 0.754(5) 0.421(5) 0.796(5) 0.028(13) Uiso 1 1 d . . . . .
H3WB H -0.464(8) 0.964(6) 0.775(6) 0.08(2) Uiso 1 1 d . . . . .
H8 H 0.309(6) 0.708(5) 0.625(5) 0.046(14) Uiso 1 1 d . . . . .
H4WA H 0.546(12) 0.878(11) 1.069(10) 0.17(5) Uiso 1 1 d . . . . .
H12A H 0.751(6) 0.612(5) 1.196(5) 0.043(16) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O9 2.065(3) 2_676 ?
Co1 O9 2.065(3) . ?
Co1 O10 2.085(3) 2_676 ?
Co1 O10 2.085(3) . ?
Co1 O1 2.107(2) . ?
Co1 O1 2.107(2) 2_676 ?
Co2 O11 2.029(3) . ?
Co2 O11 2.029(3) 2_767 ?
Co2 O4 2.104(2) 2_767 ?
Co2 O4 2.104(2) . ?
Co2 O12 2.128(3) . ?
Co2 O12 2.128(3) 2_767 ?
Co3 O13 2.055(3) . ?
Co3 O13 2.055(3) 2_667 ?
Co3 O14 2.097(3) . ?
Co3 O14 2.097(3) 2_667 ?
Co3 O5 2.124(2) . ?
Co3 O5 2.124(2) 2_667 ?
Co4 O16 2.080(3) 2_576 ?
Co4 O16 2.080(3) . ?
Co4 O8 2.085(2) 2_576 ?
Co4 O8 2.085(2) . ?
Co4 O15 2.100(3) . ?
Co4 O15 2.100(3) 2_576 ?
O8 C10 1.278(4) . ?
O1 C1 1.273(4) . ?
O5 C6 1.265(4) . ?
O4 C5 1.264(4) . ?
O3 C5 1.250(4) . ?
O12 H12B 0.89(5) . ?
O12 H12A 0.75(5) . ?
O15 H15A 0.84(5) . ?
O15 H15B 0.79(5) . ?
O16 H16B 0.85(5) . ?
O16 H16A 0.84(5) . ?
O11 H11B 0.68(5) . ?
O11 H11A 0.83(5) . ?
O6 C6 1.250(4) . ?
O2 C1 1.254(4) . ?
O14 H14A 0.84(6) . ?
O14 H14B 0.79(5) . ?
O10 H10B 0.84(6) . ?
O10 H10A 0.80(5) . ?
O9 H9B 0.88(5) . ?
O9 H9A 0.85(6) . ?
O3W H3WA 0.71(5) . ?
O3W H3WB 0.84(7) . ?
O1W H1WB 0.97(5) . ?
O1W H1WA 0.70(4) . ?
O7 C10 1.246(4) . ?
O2W H2WB 0.72(5) . ?
O2W H2WA 0.79(6) . ?
O4W H4WB 0.78(7) . ?
O4W H4WA 0.74(10) . ?
O13 H13A 0.82(4) . ?
O13 H13B 0.73(5) . ?
C7 C8 1.379(5) . ?
C7 C9 1.400(5) 2_666 ?
C7 C6 1.509(5) . ?
C4 C3 1.387(5) . ?
C4 C2 1.401(5) 2_766 ?
C4 C5 1.512(5) . ?
C8 C9 1.390(5) . ?
C8 H8 0.95(5) . ?
C3 C2 1.391(5) . ?
C3 H3 0.96(5) . ?
C1 C2 1.499(5) . ?
C10 C9 1.505(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
O9 Co1 O9 180.0 2_676 . ?
O9 Co1 O10 93.53(11) 2_676 2_676 ?
O9 Co1 O10 86.47(11) . 2_676 ?
O9 Co1 O10 86.47(11) 2_676 . ?
O9 Co1 O10 93.53(11) . . ?
O10 Co1 O10 180.00(17) 2_676 . ?
O9 Co1 O1 90.79(11) 2_676 . ?
O9 Co1 O1 89.21(11) . . ?
O10 Co1 O1 93.89(11) 2_676 . ?
O10 Co1 O1 86.11(11) . . ?
O9 Co1 O1 89.21(11) 2_676 2_676 ?
O9 Co1 O1 90.79(11) . 2_676 ?
O10 Co1 O1 86.11(11) 2_676 2_676 ?
O10 Co1 O1 93.89(11) . 2_676 ?
O1 Co1 O1 180.0 . 2_676 ?
O11 Co2 O11 180.0 . 2_767 ?
O11 Co2 O4 92.22(11) . 2_767 ?
O11 Co2 O4 87.78(11) 2_767 2_767 ?
O11 Co2 O4 87.78(11) . . ?
O11 Co2 O4 92.22(11) 2_767 . ?
O4 Co2 O4 180.0 2_767 . ?
O11 Co2 O12 86.82(13) . . ?
O11 Co2 O12 93.18(13) 2_767 . ?
O4 Co2 O12 87.19(10) 2_767 . ?
O4 Co2 O12 92.81(10) . . ?
O11 Co2 O12 93.18(13) . 2_767 ?
O11 Co2 O12 86.82(13) 2_767 2_767 ?
O4 Co2 O12 92.81(10) 2_767 2_767 ?
O4 Co2 O12 87.19(10) . 2_767 ?
O12 Co2 O12 180.0 . 2_767 ?
O13 Co3 O13 180.0(2) . 2_667 ?
O13 Co3 O14 92.67(12) . . ?
O13 Co3 O14 87.33(12) 2_667 . ?
O13 Co3 O14 87.33(12) . 2_667 ?
O13 Co3 O14 92.67(13) 2_667 2_667 ?
O14 Co3 O14 180.0 . 2_667 ?
O13 Co3 O5 87.29(11) . . ?
O13 Co3 O5 92.71(11) 2_667 . ?
O14 Co3 O5 90.70(10) . . ?
O14 Co3 O5 89.30(10) 2_667 . ?
O13 Co3 O5 92.71(11) . 2_667 ?
O13 Co3 O5 87.29(11) 2_667 2_667 ?
O14 Co3 O5 89.30(10) . 2_667 ?
O14 Co3 O5 90.70(10) 2_667 2_667 ?
O5 Co3 O5 180.0 . 2_667 ?
O16 Co4 O16 180.00(11) 2_576 . ?
O16 Co4 O8 90.05(10) 2_576 2_576 ?
O16 Co4 O8 89.95(10) . 2_576 ?
O16 Co4 O8 89.95(10) 2_576 . ?
O16 Co4 O8 90.05(10) . . ?
O8 Co4 O8 180.0 2_576 . ?
O16 Co4 O15 92.94(11) 2_576 . ?
O16 Co4 O15 87.06(11) . . ?
O8 Co4 O15 91.47(11) 2_576 . ?
O8 Co4 O15 88.53(11) . . ?
O16 Co4 O15 87.06(11) 2_576 2_576 ?
O16 Co4 O15 92.94(11) . 2_576 ?
O8 Co4 O15 88.53(11) 2_576 2_576 ?
O8 Co4 O15 91.47(11) . 2_576 ?
O15 Co4 O15 180.0 . 2_576 ?
C10 O8 Co4 131.3(2) . . ?
C1 O1 Co1 130.4(2) . . ?
C6 O5 Co3 122.5(2) . . ?
C5 O4 Co2 126.8(2) . . ?
Co2 O12 H12B 122(3) . . ?
Co2 O12 H12A 104(4) . . ?
H12B O12 H12A 111(5) . . ?
Co4 O15 H15A 116(3) . . ?
Co4 O15 H15B 112(3) . . ?
H15A O15 H15B 109(4) . . ?
Co4 O16 H16B 130(3) . . ?
Co4 O16 H16A 101(3) . . ?
H16B O16 H16A 107(4) . . ?
Co2 O11 H11B 127(4) . . ?
Co2 O11 H11A 107(3) . . ?
H11B O11 H11A 103(5) . . ?
Co3 O14 H14A 119(4) . . ?
Co3 O14 H14B 103(4) . . ?
H14A O14 H14B 99(5) . . ?
Co1 O10 H10B 121(4) . . ?
Co1 O10 H10A 118(3) . . ?
H10B O10 H10A 107(5) . . ?
Co1 O9 H9B 136(3) . . ?
Co1 O9 H9A 104(4) . . ?
H9B O9 H9A 108(5) . . ?
H3WA O3W H3WB 113(6) . . ?
H1WB O1W H1WA 103(4) . . ?
H2WB O2W H2WA 105(5) . . ?
H4WB O4W H4WA 116(8) . . ?
Co3 O13 H13A 133(3) . . ?
Co3 O13 H13B 117(4) . . ?
H13A O13 H13B 107(4) . . ?
C8 C7 C9 119.4(3) . 2_666 ?
C8 C7 C6 117.3(3) . . ?
C9 C7 C6 123.3(3) 2_666 . ?
C3 C4 C2 119.4(3) . 2_766 ?
C3 C4 C5 117.8(3) . . ?
C2 C4 C5 122.8(3) 2_766 . ?
C7 C8 C9 122.3(3) . . ?
C7 C8 H8 121(3) . . ?
C9 C8 H8 116(3) . . ?
C4 C3 C2 121.9(3) . . ?
C4 C3 H3 118(3) . . ?
C2 C3 H3 120(3) . . ?
O2 C1 O1 124.6(3) . . ?
O2 C1 C2 118.5(3) . . ?
O1 C1 C2 116.8(3) . . ?
C3 C2 C4 118.8(3) . 2_766 ?
C3 C2 C1 118.3(3) . . ?
C4 C2 C1 122.7(3) 2_766 . ?
O3 C5 O4 125.1(3) . . ?
O3 C5 C4 117.5(3) . . ?
O4 C5 C4 117.4(3) . . ?
O6 C6 O5 125.3(3) . . ?
O6 C6 C7 116.9(3) . . ?
O5 C6 C7 117.8(3) . . ?
O7 C10 O8 124.2(3) . . ?
O7 C10 C9 119.6(3) . . ?
O8 C10 C9 116.2(3) . . ?
C8 C9 C7 118.3(3) . 2_666 ?
C8 C9 C10 117.9(3) . . ?
C7 C9 C10 123.6(3) 2_666 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13A O4 0.82(4) 1.95(5) 2.772(4) 175(4) .
O1W H1WB O2W 0.97(5) 1.79(5) 2.749(5) 170(4) .
O14 H14A O4W 0.84(6) 1.86(6) 2.696(4) 173(6) .
O11 H11B O1W 0.68(5) 2.09(5) 2.750(4) 163(6) 1_645
O12 H12B O5 0.89(5) 1.91(5) 2.792(4) 171(4) 2_667
O9 H9B O8 0.88(5) 1.84(5) 2.718(4) 170(4) .
O15 H15A O3W 0.84(5) 1.90(5) 2.710(4) 161(4) .
O16 H16B O1 0.85(5) 1.90(5) 2.744(4) 170(4) 2_676
O15 H15B O3 0.79(5) 1.94(5) 2.702(4) 164(4) 1_455
O10 H10B O1W 0.84(6) 1.85(6) 2.687(4) 174(6) .
O1W H1WA O2W 0.70(4) 2.07(4) 2.773(5) 178(5) 2_577
O10 H10A O6 0.80(5) 1.93(5) 2.689(4) 159(4) .
O9 H9A O2 0.85(6) 1.82(6) 2.644(4) 163(6) .
O11 H11A O3 0.83(5) 1.87(5) 2.644(4) 155(5) 2_767
O16 H16A O7 0.84(5) 1.84(5) 2.663(4) 166(5) 2_576
O2W H2WB O15 0.72(5) 2.20(5) 2.904(4) 164(5) .
O2W H2WA O14 0.79(6) 2.05(6) 2.801(5) 161(6) 2_577
O4W H4WB O12 0.78(7) 2.04(7) 2.776(4) 159(6) .
O3W H3WA O4W 0.71(5) 2.12(5) 2.773(5) 153(5) 1_455
O14 H14B O6 0.79(5) 1.85(5) 2.595(4) 158(5) .
O13 H13B O7 0.73(5) 2.02(5) 2.731(4) 166(5) 2_666
O3W H3WB O10 0.84(7) 2.12(7) 2.935(4) 164(6) 1_455
O3W H3WB O9 0.84(7) 2.59(6) 2.987(5) 111(5) 2_576
O4W H4WA O3W 0.74(10) 2.01(11) 2.747(5) 178(11) 2_577
O12 H12A O2 0.75(5) 1.95(5) 2.696(4) 173(5) 1_556

_refine_diff_density_max         0.723
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.093


# start Validation Reply Form


_vrf_PLAT112_SOLVE_4K_a          
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem a/2 88 %Fit
RESPONSE: No additional symmetry needed, this alert may be due to the 
position of Co atom in the centre of the unit cell. PLATON ADSSYM indicated 
that P(-1) is the correct group.
;
_vrf_PLAT417_SOLVE_4K_a          
;
PROBLEM: Short Inter D-H..H-D H1WB ..H2WB . 2.10 Ang.
RESPONSE: The short non-bonding inter D-H..H-D contacts may be related to 
twinned or disordered structure. 
;
_vrf_PLAT906_SOLVE_4K_a          
;
PROBLEM: Large K Value in the Analysis of Variance ...... 9.202 Check
RESPONSE: Sometimes, in Mo K\a radiation this difference is trivial.
;
_vrf_PLAT911_SOLVE_4K_a          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 3 Report
RESPONSE: These reflections were probably affected by unexpected deviations 
in their intensities for symmetry equivalent measurements and omitted during 
initial data reduction. This is likely due to beam-stop. By using Mo radiation 
and the geometry of our goniometer, this happens quite often. Most of the 
missing reflections were excluded by the SHEL command in order to avoid 
problems related to extinction and saturation common to low theta reflections.
;


# 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_SOLVE_1U_a
_database_code_depnum_ccdc_archive 'CCDC 2288635'
loop_
_audit_author_name
_audit_author_address
'Siya T. Hulushe'
;Rhodes University
South Africa
;
_audit_update_record             
;
2024-03-11 deposited with the CCDC.	2024-04-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2016/6
_chemical_name_systematic        ?
_chemical_name_common            'dicobalt(II) pyromellitate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H Co O4'
_chemical_formula_sum            'C5 H Co O4'
_chemical_formula_weight         183.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   6.1151(7)
_cell_length_b                   17.4400(18)
_cell_length_c                   4.5477(4)
_cell_angle_alpha                90
_cell_angle_beta                 115.606(4)
_cell_angle_gamma                90
_cell_volume                     437.37(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2801
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.11
_exptl_crystal_description       prism
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.794
_exptl_crystal_F_000             360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.086
_exptl_absorpt_coefficient_mu    3.839
_shelx_estimated_absorpt_T_min   0.540
_shelx_estimated_absorpt_T_max   0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5752
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS)'
_diffrn_radiation_probe          x-ray
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-IV CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 5.26
_diffrn_reflns_number            2281
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         3.875
_diffrn_reflns_theta_max         25.110
_diffrn_reflns_theta_full        25.110
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             397
_reflns_number_gt                368
_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       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Carbon-bound H atoms were placed in calculated positions and were included in the refinement in the riding model approximation, with Uiso(H) set to 1.2 Ueq(C).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+7.1430P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         397
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0815
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_restrained_S_all      1.196
_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
Co1 Co 0.500000 0.71017(5) 1.000000 0.0122(5) Uani 1 2 d S T P . .
O2 O 0.2403(5) 0.70015(17) 0.2128(7) 0.0112(7) Uani 1 1 d . . . . .
O1 O 0.2933(6) 0.63405(17) 0.6564(7) 0.0121(7) Uani 1 1 d . . . . .
C2 C 0.0896(9) 0.5699(2) 0.1592(11) 0.0127(10) Uani 1 1 d . . . . .
C3 C 0.1743(12) 0.500000 0.3125(16) 0.0122(13) Uani 1 2 d S T P . .
H3 H 0.295271 0.500001 0.531517 0.015 Uiso 1 2 calc R U P . .
C1 C 0.2133(8) 0.6399(2) 0.3550(11) 0.0114(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.023(3) . ?
Co1 O1 2.023(3) 2_657 ?
Co1 O2 2.077(3) 8_566 ?
Co1 O2 2.077(3) 7_566 ?
Co1 O2 2.195(3) 1_556 ?
Co1 O2 2.195(3) 2_656 ?
O2 C1 1.281(5) . ?
O1 C1 1.245(5) . ?
C2 C2 1.388(10) 2 ?
C2 C3 1.389(5) . ?
C2 C1 1.507(6) . ?
C3 H3 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 97.99(18) . 2_657 ?
O1 Co1 O2 159.07(12) . 8_566 ?
O1 Co1 O2 93.11(12) 2_657 8_566 ?
O1 Co1 O2 93.11(12) . 7_566 ?
O1 Co1 O2 159.07(12) 2_657 7_566 ?
O2 Co1 O2 82.28(17) 8_566 7_566 ?
O1 Co1 O2 87.64(12) . 1_556 ?
O1 Co1 O2 86.37(12) 2_657 1_556 ?
O2 Co1 O2 110.82(12) 8_566 1_556 ?
O2 Co1 O2 76.38(13) 7_566 1_556 ?
O1 Co1 O2 86.37(12) . 2_656 ?
O1 Co1 O2 87.64(12) 2_657 2_656 ?
O2 Co1 O2 76.38(13) 8_566 2_656 ?
O2 Co1 O2 110.82(12) 7_566 2_656 ?
O2 Co1 O2 170.87(16) 1_556 2_656 ?
C1 O2 Co1 129.3(3) . 7_566 ?
C1 O2 Co1 124.3(3) . 1_554 ?
Co1 O2 Co1 103.62(12) 7_566 1_554 ?
C1 O1 Co1 127.9(3) . . ?
C2 C2 C3 118.6(3) 2 . ?
C2 C2 C1 125.8(2) 2 . ?
C3 C2 C1 115.6(4) . . ?
C2 C3 C2 122.8(6) . 6_565 ?
C2 C3 H3 118.6 . . ?
C2 C3 H3 118.6 6_565 . ?
O1 C1 O2 123.2(4) . . ?
O1 C1 C2 116.2(4) . . ?
O2 C1 C2 120.5(4) . . ?

_refine_diff_density_max         0.859
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.147



# start Validation Reply Form



_vrf_PLAT088_SOLVE_1U_a          
;
PROBLEM: Poor Data / Parameter Ratio ........8.10 Note
RESPONSE: The reflection to parameter ratio is low due to very large number 
of refined parameters and the very weakly diffracting nature of the crystals. 
;
_vrf_PLAT430_SOLVE_1U_a          
;
PROBLEM: Short Inter D...A Contact O2 ..O2 . 2.64 Ang.
RESPONSE: The short interaction is a consequence of distortion in the 
octahedral geometry exhibited by the cobalt(II) coordination sphere. 
Additionally, this distortion is indicated by huge bond angle deviations 
from 90 degrees. For a structure with marginal or no distortion, these 
angles should be close or equal to 90 and 180 degrees.
;


# 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_SOLVE_4M_a
_database_code_depnum_ccdc_archive 'CCDC 2288636'
loop_
_audit_author_name
_audit_author_address
'Siya T. Hulushe'
;Rhodes University
South Africa
;
_audit_update_record             
;
2024-03-11 deposited with the CCDC.	2024-04-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2016/6
_chemical_name_systematic        ?
_chemical_name_common            'dicobalt(II) pyromellitate dihydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H3 Co O5'
_chemical_formula_sum            'C5 H3 Co O5'
_chemical_formula_weight         202.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   3.3576(6)
_cell_length_b                   9.0091(16)
_cell_length_c                   9.5434(15)
_cell_angle_alpha                113.881(5)
_cell_angle_beta                 99.313(6)
_cell_angle_gamma                93.915(6)
_cell_volume                     257.60(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3171
_cell_measurement_theta_min      2.386
_cell_measurement_theta_max      24.40
_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_density_diffrn    2.604
_exptl_crystal_F_000             200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.074
_exptl_absorpt_coefficient_mu    3.286
_shelx_estimated_absorpt_T_min   0.489
_shelx_estimated_absorpt_T_max   0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5608
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction.
wR2(int) was 0.1117 before and 0.0891 after correction.
The Ratio of minimum to maximum transmission is 0.7525.
The λ/2 correction factor is Not present.
;
_diffrn_radiation_probe          x-ray
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-IV CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.54
_diffrn_reflns_number            11857
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.386
_diffrn_reflns_theta_max         25.369
_diffrn_reflns_theta_full        25.125
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             927
_reflns_number_gt                695
_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       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Carbon-bound H atoms were placed in calculated positions and were included in
the refinement in the riding model approximation, with Uiso(H) set to
1.2 Ueq(C).

The H atoms of the water molecules were located on a difference Fourier map and
refined with the O---H bond lengths and the H---O---H bond angles restrained to
0.84 Å and 109 ° respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0405P)²+2.8013P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         927
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1434
_refine_ls_wR_factor_gt          0.1275
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Co1 Co 0.000000 1.000000 0.500000 0.0358(5) Uani 1 2 d S . P . .
Co2 Co 0.500000 0.500000 0.000000 0.0365(5) Uani 1 2 d S . P . .
O2 O 0.0609(17) 0.5491(7) 0.1533(6) 0.0373(13) Uani 1 1 d . . . . .
O4 O 0.4735(17) 0.0473(7) 0.3865(7) 0.0385(14) Uani 1 1 d . . . . .
O3 O 0.6230(18) 0.1121(7) 0.1991(7) 0.0405(14) Uani 1 1 d . . . . .
O5W O 0.5325(18) 0.7424(7) 0.0270(7) 0.0422(14) Uani 1 1 d . . . . .
H5WA H 0.539842 0.805633 0.122285 0.063 Uiso 1 1 d R U . . .
H5WB H 0.322861 0.751536 -0.030594 0.063 Uiso 1 1 d R U . . .
O1 O -0.0722(17) 0.7663(7) 0.3456(6) 0.0362(13) Uani 1 1 d . . . . .
C4 C 0.530(2) 0.3305(10) 0.4269(9) 0.0330(18) Uani 1 1 d . . . . .
C2 C 0.320(2) 0.5793(10) 0.4111(9) 0.0315(17) Uani 1 1 d . . . . .
C1 C 0.100(2) 0.6419(10) 0.2991(10) 0.0336(18) Uani 1 1 d . . . . .
C3 C 0.359(2) 0.4134(10) 0.3427(9) 0.0340(18) Uani 1 1 d . . . . .
H3 H 0.262691 0.353929 0.232826 0.041 Uiso 1 1 calc R U . . .
C5 C 0.549(2) 0.1528(10) 0.3290(10) 0.0345(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 1.992(5) 2_576 ?
Co1 O1 1.992(5) . ?
Co1 O4 2.082(5) 2_666 ?
Co1 O4 2.082(5) 1_465 ?
Co1 O4 2.173(6) 2_566 ?
Co1 O4 2.173(6) 1_565 ?
Co2 O5W 2.086(6) 2_665 ?
Co2 O5W 2.086(6) . ?
Co2 O2 2.087(5) 2_565 ?
Co2 O2 2.087(5) 1_655 ?
Co2 O2 2.185(6) 2_665 ?
Co2 O2 2.185(6) . ?
O2 C1 1.279(10) . ?
O4 C5 1.305(10) . ?
O3 C5 1.216(10) . ?
O5W H5WA 0.8507 . ?
O5W H5WB 0.8506 . ?
O1 C1 1.248(9) . ?
C4 C3 1.390(10) . ?
C4 C2 1.407(11) 2_666 ?
C4 C5 1.504(11) . ?
C2 C3 1.393(11) . ?
C2 C1 1.514(10) . ?
C3 H3 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 180.0 2_576 . ?
O1 Co1 O4 93.5(2) 2_576 2_666 ?
O1 Co1 O4 86.5(2) . 2_666 ?
O1 Co1 O4 86.5(2) 2_576 1_465 ?
O1 Co1 O4 93.5(2) . 1_465 ?
O4 Co1 O4 180.0 2_666 1_465 ?
O1 Co1 O4 87.1(2) 2_576 2_566 ?
O1 Co1 O4 92.9(2) . 2_566 ?
O4 Co1 O4 104.2(2) 2_666 2_566 ?
O4 Co1 O4 75.8(2) 1_465 2_566 ?
O1 Co1 O4 92.9(2) 2_576 1_565 ?
O1 Co1 O4 87.1(2) . 1_565 ?
O4 Co1 O4 75.8(2) 2_666 1_565 ?
O4 Co1 O4 104.2(2) 1_465 1_565 ?
O4 Co1 O4 180.0 2_566 1_565 ?
O5W Co2 O5W 180.0 2_665 . ?
O5W Co2 O2 92.4(2) 2_665 2_565 ?
O5W Co2 O2 87.6(2) . 2_565 ?
O5W Co2 O2 87.6(2) 2_665 1_655 ?
O5W Co2 O2 92.4(2) . 1_655 ?
O2 Co2 O2 180.0(3) 2_565 1_655 ?
O5W Co2 O2 88.8(2) 2_665 2_665 ?
O5W Co2 O2 91.2(2) . 2_665 ?
O2 Co2 O2 103.6(2) 2_565 2_665 ?
O2 Co2 O2 76.4(2) 1_655 2_665 ?
O5W Co2 O2 91.2(2) 2_665 . ?
O5W Co2 O2 88.8(2) . . ?
O2 Co2 O2 76.4(2) 2_565 . ?
O2 Co2 O2 103.6(2) 1_655 . ?
O2 Co2 O2 180.0 2_665 . ?
C1 O2 Co2 120.2(5) . 1_455 ?
C1 O2 Co2 131.4(5) . . ?
Co2 O2 Co2 103.6(2) 1_455 . ?
C5 O4 Co1 112.9(5) . 1_645 ?
C5 O4 Co1 134.5(5) . 1_545 ?
Co1 O4 Co1 104.2(2) 1_645 1_545 ?
Co2 O5W H5WA 109.5 . . ?
Co2 O5W H5WB 109.2 . . ?
H5WA O5W H5WB 109.4 . . ?
C1 O1 Co1 144.1(5) . . ?
C3 C4 C2 117.8(7) . 2_666 ?
C3 C4 C5 114.5(7) . . ?
C2 C4 C5 127.6(7) 2_666 . ?
C3 C2 C4 118.8(7) . 2_666 ?
C3 C2 C1 114.5(7) . . ?
C4 C2 C1 126.7(7) 2_666 . ?
O1 C1 O2 121.8(7) . . ?
O1 C1 C2 121.9(7) . . ?
O2 C1 C2 115.8(7) . . ?
C4 C3 C2 123.4(7) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
O3 C5 O4 122.5(8) . . ?
O3 C5 C4 119.4(7) . . ?
O4 C5 C4 118.1(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5W H5WA O4 0.85 2.64 3.467(8) 165.6 1_565
O5W H5WA O3 0.85 2.53 3.025(8) 117.7 1_565
O5W H5WA O1 0.85 2.48 3.030(8) 123.3 1_655
O5W H5WB O3 0.85 2.41 2.944(8) 121.7 2_665

_refine_diff_density_max         0.763
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.145



# start Validation Reply Form



_vrf_PLAT088_SOLVE_4M_a          
;
PROBLEM: Poor Data / Parameter Ratio ........8.91 Note
RESPONSE: The reflection to parameter ratio is low due to low symmetry of 
the structure (P-1), very large number of refined parameters and the very 
weakly diffracting nature of the crystals (after they were subjected to
both low pressure heating and rehydration).
;
_vrf_PLAT341_SOLVE_4M_a          
;
PROBLEM: Low Bond Precision on C-C Bonds.........0.0118 Ang.
RESPONSE: This alert is generated because the crystal(s) diffracted 
extremely weak and low pressure heating induced disorder in the atom 
positions. Multiple attempts were made to generate better diffracting 
crystals.
;
_vrf_PLAT430_SOLVE_4M_a          
;
PROBLEM: Short Inter D...A Contact O4 ..O4 . 2.62 Ang.
RESPONSE: The short interaction is a consequence of distortion in the 
octahedral geometry exhibited by the Co1 coordination sphere. This results 
in O4 oxygen atoms to be in close proximity, and hence the short interactions. 
Additionally, the distortion is indicated by huge bond angle deviations from 
90 degrees. For a structure with marginal or no distortion, these angles 
should be close or equal to 90 and 180 degrees.
;
_vrf_PLAT906_SOLVE_4M_a          
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.991 Check 
RESPONSE: Sometimes, in Mo K\a radiation this difference is trivial.
;
_vrf_PLAT911_SOLVE_4M_a          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report 
RESPONSE: These reflections were probably affected by unexpected deviations 
in their intensities for symmetry equivalent measurements and omitted during 
initial data reduction. This is likely due to beam-stop. By using Mo radiation 
and the geometry of our goniometer, this happens quite often. Most of the 
missing reflections were excluded by the SHEL command in order to avoid 
problems related to extinction and saturation common to low theta reflections.
;


# end Validation Reply Form

