# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2016

####################################################################### 
# 
# 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_ZnMT
_database_code_depnum_ccdc_archive 'CCDC 1408922'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        'Tetra-aqua-bis(hydrogen maleato)-zinc(ii)'
_chemical_name_common            'zinc maleate tetrahydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         Zn(H2O)4(C4O4H3)2
_chemical_formula_sum            'C8 H14 O12 Zn'
_chemical_formula_weight         367.56

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'
Zn Zn 0.2839 1.4301 '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                   5.1749(2)
_cell_length_b                   7.2736(3)
_cell_length_c                   9.1901(4)
_cell_angle_alpha                108.304(2)
_cell_angle_beta                 105.213(2)
_cell_angle_gamma                92.434(2)
_cell_volume                     313.95(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_F_000             188
_exptl_transmission_factor_min   0.6641
_exptl_transmission_factor_max   0.7482
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.023
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34723
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.440
_diffrn_reflns_theta_max         41.471
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4197
_reflns_number_gt                3997
_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 APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_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)+(0.0353P)²+0.0490P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         4197
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0630
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.001
_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
Zn01 Zn 0.5000 0.5000 1.0000 0.01019(3) Uani 1 2 d S . P . .
O002 O 0.82089(10) 0.36413(8) 1.10097(6) 0.01213(8) Uani 1 1 d . . . . .
O003 O 0.24869(11) 0.24330(8) 0.92469(6) 0.01317(8) Uani 1 1 d . . . . .
O004 O 0.64524(10) 0.43994(8) 0.79507(6) 0.01256(8) Uani 1 1 d . . . . .
O005 O 0.29916(12) 0.22537(10) 0.61804(7) 0.01735(10) Uani 1 1 d . . . . .
O006 O 0.15844(12) 0.04008(10) 0.33339(7) 0.01798(10) Uani 1 1 d . . . . .
O007 O 0.30331(13) 0.02100(9) 0.12367(7) 0.01662(9) Uani 1 1 d . . . . .
C008 C 0.52645(12) 0.32772(9) 0.65501(7) 0.01047(9) Uani 1 1 d . . . . .
C009 C 0.33433(13) 0.08868(9) 0.26928(8) 0.01166(9) Uani 1 1 d . . . . .
C00A C 0.58515(13) 0.22593(10) 0.37203(8) 0.01280(10) Uani 1 1 d . . . . .
C00B C 0.66666(13) 0.32218(10) 0.53098(8) 0.01257(9) Uani 1 1 d . . . . .
H1 H 0.196(4) 0.185(3) 0.841(2) 0.030(4) Uiso 1 1 d . . . . .
H2 H 0.280(4) 0.167(3) 0.970(2) 0.027(4) Uiso 1 1 d . . . . .
H3 H 0.818(4) 0.262(2) 1.035(2) 0.024(4) Uiso 1 1 d . . . . .
H4 H 0.966(3) 0.419(2) 1.1255(19) 0.020(3) Uiso 1 1 d . . . . .
H5 H 0.223(5) 0.110(4) 0.454(3) 0.062(7) Uiso 1 1 d . . . . .
H6 H 0.696(3) 0.242(2) 0.3139(19) 0.019(3) Uiso 1 1 d . . . . .
H7 H 0.831(3) 0.406(2) 0.576(2) 0.023(4) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn01 0.00954(4) 0.01129(5) 0.01054(5) 0.00388(3) 0.00403(3) 0.00118(3)
O002 0.01082(17) 0.01284(18) 0.01242(19) 0.00343(15) 0.00384(14) 0.00177(14)
O003 0.01488(19) 0.01255(19) 0.00978(18) 0.00237(15) 0.00205(14) -0.00182(15)
O004 0.01227(18) 0.01513(19) 0.00827(17) 0.00119(14) 0.00326(14) 0.00014(15)
O005 0.01373(19) 0.0243(3) 0.01054(19) 0.00108(17) 0.00485(15) -0.00571(18)
O006 0.0160(2) 0.0237(3) 0.00962(19) 0.00064(17) 0.00361(16) -0.00596(18)
O007 0.0251(2) 0.0147(2) 0.00812(18) 0.00175(15) 0.00478(17) -0.00051(18)
C008 0.0104(2) 0.0119(2) 0.0089(2) 0.00263(16) 0.00352(16) 0.00146(16)
C009 0.0145(2) 0.0111(2) 0.0088(2) 0.00270(17) 0.00328(17) 0.00185(17)
C00A 0.0136(2) 0.0145(2) 0.0102(2) 0.00268(18) 0.00537(18) 0.00065(18)
C00B 0.0111(2) 0.0154(2) 0.0102(2) 0.00218(18) 0.00440(17) -0.00042(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
Zn01 O003 2.0411(5) 2_667 ?
Zn01 O003 2.0411(5) . ?
Zn01 O002 2.1217(5) 2_667 ?
Zn01 O002 2.1218(5) . ?
Zn01 O004 2.1346(5) 2_667 ?
Zn01 O004 2.1346(5) . ?
O002 H3 0.796(18) . ?
O002 H4 0.776(16) . ?
O003 H1 0.724(18) . ?
O003 H2 0.792(19) . ?
O004 C008 1.2582(8) . ?
O005 C008 1.2689(8) . ?
O005 H5 1.41(3) . ?
O006 C009 1.2983(9) . ?
O006 H5 1.02(3) . ?
O007 C009 1.2352(8) . ?
C008 C00B 1.4950(9) . ?
C009 C00A 1.4925(9) . ?
C00A C00B 1.3458(9) . ?
C00A H6 0.908(17) . ?
C00B H7 0.940(17) . ?

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
O003 Zn01 O003 180.0 2_667 . ?
O003 Zn01 O002 89.10(2) 2_667 2_667 ?
O003 Zn01 O002 90.90(2) . 2_667 ?
O003 Zn01 O002 90.90(2) 2_667 . ?
O003 Zn01 O002 89.10(2) . . ?
O002 Zn01 O002 180.0 2_667 . ?
O003 Zn01 O004 96.97(2) 2_667 2_667 ?
O003 Zn01 O004 83.03(2) . 2_667 ?
O002 Zn01 O004 87.78(2) 2_667 2_667 ?
O002 Zn01 O004 92.22(2) . 2_667 ?
O003 Zn01 O004 83.03(2) 2_667 . ?
O003 Zn01 O004 96.97(2) . . ?
O002 Zn01 O004 92.21(2) 2_667 . ?
O002 Zn01 O004 87.78(2) . . ?
O004 Zn01 O004 180.0 2_667 . ?
Zn01 O002 H3 107.1(13) . . ?
Zn01 O002 H4 116.7(12) . . ?
H3 O002 H4 106.3(17) . . ?
Zn01 O003 H1 122.0(15) . . ?
Zn01 O003 H2 120.3(13) . . ?
H1 O003 H2 105.1(19) . . ?
C008 O004 Zn01 127.20(4) . . ?
C008 O005 H5 109.6(11) . . ?
C009 O006 H5 109.1(15) . . ?
O004 C008 O005 122.92(6) . . ?
O004 C008 C00B 116.21(6) . . ?
O005 C008 C00B 120.86(6) . . ?
O007 C009 O006 121.67(6) . . ?
O007 C009 C00A 118.10(6) . . ?
O006 C009 C00A 120.21(6) . . ?
C00B C00A C009 130.39(6) . . ?
C00B C00A H6 117.9(10) . . ?
C009 C00A H6 111.7(10) . . ?
C00A C00B C008 129.92(6) . . ?
C00A C00B H7 119.0(10) . . ?
C008 C00B H7 111.0(10) . . ?

_refine_diff_density_max         1.666
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.099

_shelxl_version_number           2014/6

_shelx_res_file                  
;
TITL mo_matrix_0m_AB_a.res in P-1
CELL  0.71073   5.1749   7.2736   9.1901  108.304  105.213   92.434
ZERR    1.000   0.0002   0.0003   0.0004    0.002    0.002    0.002
LATT 1
SFAC C  H  O  Zn
UNIT 8  14  12  1
REM Old TITL mo_matrix_0m_AB in P-1
REM SHELXT solution in P-1
REM R1 0.046,  Rweak 0.013,  Alpha 0.071,  Orientation as input
REM Formula found by SHELXT:  C8 O12 Zn
L.S. 50
ACTA
BOND $H
FMAP 2
PLAN 2
TEMP -183.000
WGHT    0.035300    0.049000
FVAR       0.94744
ZN01  4    0.500000    0.500000    1.000000    10.50000    0.00954    0.01129 =
         0.01054    0.00388    0.00403    0.00118
O002  3    0.820895    0.364132    1.100966    11.00000    0.01082    0.01284 =
         0.01242    0.00343    0.00384    0.00177
O003  3    0.248687    0.243300    0.924694    11.00000    0.01488    0.01255 =
         0.00978    0.00237    0.00205   -0.00182
O004  3    0.645239    0.439944    0.795073    11.00000    0.01227    0.01513 =
         0.00827    0.00119    0.00326    0.00014
O005  3    0.299161    0.225368    0.618042    11.00000    0.01373    0.02428 =
         0.01054    0.00108    0.00485   -0.00571
O006  3    0.158435    0.040077    0.333390    11.00000    0.01601    0.02375 =
         0.00962    0.00064    0.00361   -0.00596
O007  3    0.303309    0.021004    0.123666    11.00000    0.02515    0.01472 =
         0.00812    0.00175    0.00478   -0.00051
C008  1    0.526449    0.327719    0.655015    11.00000    0.01039    0.01194 =
         0.00886    0.00263    0.00352    0.00146
C009  1    0.334327    0.088678    0.269285    11.00000    0.01453    0.01113 =
         0.00879    0.00270    0.00328    0.00185
C00A  1    0.585154    0.225935    0.372028    11.00000    0.01362    0.01454 =
         0.01018    0.00268    0.00537    0.00065
C00B  1    0.666656    0.322176    0.530983    11.00000    0.01113    0.01545 =
         0.01016    0.00218    0.00440   -0.00042
H1    2    0.195627    0.184703    0.840764    11.00000    0.02959
H2    2    0.280008    0.166965    0.970250    11.00000    0.02660
H3    2    0.817588    0.261519    1.034974    11.00000    0.02447
H4    2    0.966075    0.418837    1.125520    11.00000    0.01976
H5    2    0.223474    0.109992    0.453905    11.00000    0.06160
H6    2    0.696253    0.242379    0.313945    11.00000    0.01920
H7    2    0.831204    0.406438    0.576149    11.00000    0.02314
HKLF 4

REM  mo_matrix_0m_AB_a.res in P-1
REM R1 =  0.0260 for    3997 Fo > 4sig(Fo)  and  0.0290 for all    4197 data
REM    125 parameters refined using      0 restraints

END

WGHT      0.0353      0.0490

REM Highest difference peak  1.666,  deepest hole -0.641,  1-sigma level  0.099
Q1    1   0.4723  0.4973  0.9354  11.00000  0.05    1.67
Q2    1   0.4140  0.4581  1.0019  11.00000  0.05    1.03
;
_shelx_res_checksum              35739

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
####################################################################### 
# 
# 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_NiMT
_database_code_depnum_ccdc_archive 'CCDC 1408923'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        'Tetra-aqua-bis(hydrogen maleato)-nickel(ii)'
_chemical_name_common            'nickel maleate tetrahydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         Ni(H2O)4(C4O4H3)2
_chemical_formula_sum            'C8 H14 Ni O12'
_chemical_formula_weight         360.90

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'
Ni Ni 0.3393 1.1124 '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                   5.1420(3)
_cell_length_b                   7.2793(4)
_cell_length_c                   9.1121(5)
_cell_angle_alpha                108.025(3)
_cell_angle_beta                 105.191(3)
_cell_angle_gamma                92.140(3)
_cell_volume                     310.38(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_F_000             186
_exptl_transmission_factor_min   0.6158
_exptl_transmission_factor_max   0.7479
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.631
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            24601
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.454
_diffrn_reflns_theta_max         40.061
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3783
_reflns_number_gt                3346
_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 APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_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)+(0.0379P)²+0.0413P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         3783
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0751
_refine_ls_wR_factor_gt          0.0722
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
Ni01 Ni 0.5000 0.5000 1.0000 0.01037(5) Uani 1 2 d S . P . .
O002 O 0.81718(13) 0.36536(11) 1.09924(9) 0.01332(11) Uani 1 1 d . . . . .
O003 O 0.24621(14) 0.24889(10) 0.92567(9) 0.01358(11) Uani 1 1 d . . . . .
O004 O 0.64126(13) 0.44094(10) 0.79827(8) 0.01331(11) Uani 1 1 d . . . . .
O005 O 0.31091(16) 0.02039(11) 0.12443(9) 0.01787(13) Uani 1 1 d . . . . .
O006 O 0.15838(15) 0.04084(12) 0.33365(9) 0.02007(14) Uani 1 1 d . . . . .
O007 O 0.29730(15) 0.22468(12) 0.62066(9) 0.01891(14) Uani 1 1 d . . . . .
C008 C 0.33799(18) 0.08928(13) 0.27003(11) 0.01321(14) Uani 1 1 d . . . . .
C009 C 0.52374(16) 0.32813(13) 0.65780(10) 0.01166(13) Uani 1 1 d . . . . .
C00A C 0.66582(17) 0.32388(14) 0.53321(11) 0.01404(14) Uani 1 1 d . . . . .
C00B C 0.58722(18) 0.22774(14) 0.37385(11) 0.01428(14) Uani 1 1 d . . . . .
H1 H 0.828(4) 0.406(3) 0.576(2) 0.025(4) Uiso 1 1 d . . . . .
H2 H 0.708(3) 0.241(2) 0.3165(19) 0.015(3) Uiso 1 1 d . . . . .
H3 H 0.203(4) 0.192(3) 0.833(3) 0.041(6) Uiso 1 1 d . . . . .
H4 H 0.280(4) 0.174(3) 0.974(2) 0.024(4) Uiso 1 1 d . . . . .
H5 H 0.204(6) 0.107(4) 0.449(4) 0.068(8) Uiso 1 1 d . . . . .
H6 H 0.959(4) 0.423(3) 1.118(2) 0.029(5) Uiso 1 1 d . . . . .
H7 H 0.816(4) 0.262(3) 1.034(3) 0.033(5) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni01 0.00737(6) 0.01285(7) 0.00936(7) 0.00216(5) 0.00198(5) -0.00096(4)
O002 0.0096(2) 0.0148(3) 0.0140(3) 0.0031(2) 0.0029(2) 0.0003(2)
O003 0.0130(3) 0.0134(3) 0.0110(3) 0.0016(2) 0.0016(2) -0.0026(2)
O004 0.0106(2) 0.0165(3) 0.0097(3) 0.0012(2) 0.0020(2) -0.0012(2)
O005 0.0231(3) 0.0175(3) 0.0099(3) 0.0015(2) 0.0038(2) -0.0016(2)
O006 0.0153(3) 0.0271(4) 0.0116(3) -0.0004(3) 0.0030(2) -0.0078(2)
O007 0.0128(3) 0.0273(4) 0.0117(3) 0.0008(2) 0.0035(2) -0.0080(2)
C008 0.0137(3) 0.0133(3) 0.0107(3) 0.0026(3) 0.0022(3) 0.0007(2)
C009 0.0095(3) 0.0139(3) 0.0103(3) 0.0029(2) 0.0022(2) 0.0005(2)
C00A 0.0102(3) 0.0175(4) 0.0123(3) 0.0022(3) 0.0033(3) -0.0019(3)
C00B 0.0127(3) 0.0169(4) 0.0118(3) 0.0026(3) 0.0041(3) -0.0009(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
Ni01 O003 2.0237(7) 2_667 ?
Ni01 O003 2.0237(7) . ?
Ni01 O004 2.0798(7) . ?
Ni01 O004 2.0798(7) 2_667 ?
Ni01 O002 2.0816(7) 2_667 ?
Ni01 O002 2.0816(7) . ?
O002 H6 0.78(2) . ?
O002 H7 0.80(2) . ?
O003 H3 0.78(2) . ?
O003 H4 0.799(19) . ?
O004 C009 1.2589(11) . ?
O005 C008 1.2318(11) . ?
O006 C008 1.3024(12) . ?
O006 H5 0.97(3) . ?
O007 C009 1.2679(11) . ?
O007 H5 1.47(3) . ?
C008 C00B 1.4937(13) . ?
C009 C00A 1.4961(13) . ?
C00A C00B 1.3432(13) . ?
C00A H1 0.923(18) . ?
C00B H2 0.929(16) . ?

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
O003 Ni01 O003 180.0 2_667 . ?
O003 Ni01 O004 82.93(3) 2_667 . ?
O003 Ni01 O004 97.07(3) . . ?
O003 Ni01 O004 97.07(3) 2_667 2_667 ?
O003 Ni01 O004 82.93(3) . 2_667 ?
O004 Ni01 O004 180.0 . 2_667 ?
O003 Ni01 O002 89.74(3) 2_667 2_667 ?
O003 Ni01 O002 90.26(3) . 2_667 ?
O004 Ni01 O002 92.29(3) . 2_667 ?
O004 Ni01 O002 87.71(3) 2_667 2_667 ?
O003 Ni01 O002 90.26(3) 2_667 . ?
O003 Ni01 O002 89.74(3) . . ?
O004 Ni01 O002 87.71(3) . . ?
O004 Ni01 O002 92.29(3) 2_667 . ?
O002 Ni01 O002 180.00(3) 2_667 . ?
Ni01 O002 H6 112.4(14) . . ?
Ni01 O002 H7 108.0(15) . . ?
H6 O002 H7 106(2) . . ?
Ni01 O003 H3 116.0(16) . . ?
Ni01 O003 H4 118.6(13) . . ?
H3 O003 H4 109(2) . . ?
C009 O004 Ni01 127.52(6) . . ?
C008 O006 H5 112.6(17) . . ?
C009 O007 H5 112.3(11) . . ?
O005 C008 O006 121.47(8) . . ?
O005 C008 C00B 118.19(8) . . ?
O006 C008 C00B 120.33(8) . . ?
O004 C009 O007 123.21(8) . . ?
O004 C009 C00A 115.92(7) . . ?
O007 C009 C00A 120.87(8) . . ?
C00B C00A C009 130.00(8) . . ?
C00B C00A H1 117.9(11) . . ?
C009 C00A H1 112.1(11) . . ?
C00A C00B C008 130.49(8) . . ?
C00A C00B H2 117.1(10) . . ?
C008 C00B H2 112.3(10) . . ?

_refine_diff_density_max         1.004
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.104

_shelxl_version_number           2014/6

_shelx_res_file                  
;
TITL mo_matrix_0m_a.res in P-1
CELL  0.71073   5.1420   7.2793   9.1121  108.025  105.191   92.140
ZERR    1.000   0.0003   0.0004   0.0005    0.003    0.003    0.003
LATT 1
SFAC C  H  O  Ni
UNIT 8  14  12  1
REM Old TITL mo_matrix_0m in P-1
REM SHELXT solution in P-1
REM R1 0.057,  Rweak 0.008,  Alpha 0.068,  Orientation as input
REM Formula found by SHELXT:  C8 O12 Ni
L.S. 50
ACTA
BOND $H
FMAP 2
PLAN 5
TEMP -183.000
WGHT    0.037900    0.041300
FVAR       1.00321
NI01  4    0.500000    0.500000    1.000000    10.50000    0.00737    0.01285 =
         0.00936    0.00216    0.00198   -0.00096
O002  3    0.817177    0.365362    1.099238    11.00000    0.00956    0.01485 =
         0.01395    0.00314    0.00286    0.00026
O003  3    0.246212    0.248885    0.925673    11.00000    0.01303    0.01345 =
         0.01103    0.00160    0.00161   -0.00259
O004  3    0.641258    0.440941    0.798267    11.00000    0.01064    0.01652 =
         0.00970    0.00122    0.00201   -0.00124
O005  3    0.310907    0.020386    0.124425    11.00000    0.02315    0.01749 =
         0.00986    0.00146    0.00381   -0.00156
O006  3    0.158375    0.040844    0.333652    11.00000    0.01525    0.02707 =
         0.01160   -0.00037    0.00297   -0.00777
O007  3    0.297300    0.224684    0.620656    11.00000    0.01275    0.02728 =
         0.01173    0.00077    0.00352   -0.00797
C008  1    0.337992    0.089284    0.270033    11.00000    0.01370    0.01333 =
         0.01071    0.00256    0.00222    0.00071
C009  1    0.523744    0.328131    0.657805    11.00000    0.00949    0.01393 =
         0.01029    0.00287    0.00223    0.00046
C00A  1    0.665822    0.323882    0.533213    11.00000    0.01015    0.01750 =
         0.01228    0.00224    0.00335   -0.00193
C00B  1    0.587221    0.227741    0.373849    11.00000    0.01269    0.01689 =
         0.01184    0.00262    0.00412   -0.00091
H1    2    0.828383    0.405546    0.576153    11.00000    0.02532
H2    2    0.707683    0.241474    0.316524    11.00000    0.01519
H3    2    0.203089    0.191571    0.833046    11.00000    0.04072
H4    2    0.280462    0.173634    0.973747    11.00000    0.02446
H5    2    0.204490    0.107324    0.449107    11.00000    0.06823
H6    2    0.959430    0.423264    1.117635    11.00000    0.02927
H7    2    0.815761    0.262375    1.033627    11.00000    0.03348
HKLF 4

REM  mo_matrix_0m_a.res in P-1
REM R1 =  0.0321 for    3346 Fo > 4sig(Fo)  and  0.0398 for all    3783 data
REM    125 parameters refined using      0 restraints

END

WGHT      0.0379      0.0413

REM Highest difference peak  1.004,  deepest hole -0.971,  1-sigma level  0.104
Q1    1   0.4598  0.4838  0.9259  11.00000  0.05    1.00
Q2    1   0.4780  0.5745  0.9492  11.00000  0.05    0.89
Q3    1   0.4370  0.5855  1.0140  11.00000  0.05    0.82
Q4    1   0.5902  0.3371  0.5982  11.00000  0.05    0.71
Q5    1   0.6185  0.2765  0.4481  11.00000  0.05    0.68
;
_shelx_res_checksum              91422

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_CoMT
_database_code_depnum_ccdc_archive 'CCDC 1408924'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        'Tetra-aqua-bis(hydrogen maleato)-cobalt(ii)'
_chemical_name_common            'cobalt maleate tetrahydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         Co(H2O)4(C4O4H3)2
_chemical_formula_sum            'C8 H14 Co O12'
_chemical_formula_weight         361.12

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                   5.1742(3)
_cell_length_b                   7.2742(4)
_cell_length_c                   9.2053(5)
_cell_angle_alpha                108.809(2)
_cell_angle_beta                 105.003(2)
_cell_angle_gamma                92.409(3)
_cell_volume                     313.79(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_F_000             185
_exptl_transmission_factor_min   0.6994
_exptl_transmission_factor_max   0.7476
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.434
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55628
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.441
_diffrn_reflns_theta_max         46.633
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5537
_reflns_number_gt                4888
_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 APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'

_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+0.0398P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         5537
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0597
_refine_ls_wR_factor_gt          0.0565
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
Co01 Co 0.5000 0.5000 1.0000 0.00851(2) Uani 1 2 d S . P . .
O002 O 0.17818(9) 0.63439(6) 0.89772(5) 0.01171(6) Uani 1 1 d . . . . .
O003 O 0.74730(9) 0.75861(6) 1.07512(5) 0.01276(7) Uani 1 1 d . . . . .
O004 O 0.64212(9) 0.43911(6) 0.79495(5) 0.01186(6) Uani 1 1 d . . . . .
O005 O 0.15729(10) 0.03710(8) 0.33240(6) 0.01689(8) Uani 1 1 d . . . . .
O006 O 0.29579(10) 0.22438(8) 0.61678(6) 0.01641(8) Uani 1 1 d . . . . .
O007 O 0.29912(11) 0.02123(7) 0.12209(5) 0.01560(7) Uani 1 1 d . . . . .
C008 C 0.33166(11) 0.08760(8) 0.26820(6) 0.01109(7) Uani 1 1 d . . . . .
C009 C 0.52345(10) 0.32694(8) 0.65430(6) 0.01001(7) Uani 1 1 d . . . . .
C00A C 0.66460(11) 0.32137(8) 0.53052(7) 0.01183(8) Uani 1 1 d . . . . .
C00B C 0.58296(11) 0.22520(8) 0.37125(6) 0.01212(8) Uani 1 1 d . . . . .
H1 H 0.177(3) 0.737(2) 0.9600(19) 0.030(3) Uiso 1 1 d . . . . .
H2 H 0.029(3) 0.579(2) 0.8753(17) 0.025(3) Uiso 1 1 d . . . . .
H3 H 0.824(4) 0.818(3) 1.164(2) 0.042(4) Uiso 1 1 d . . . . .
H4 H 0.717(3) 0.831(2) 1.0243(19) 0.033(4) Uiso 1 1 d . . . . .
H5 H 0.833(3) 0.404(2) 0.5742(17) 0.026(3) Uiso 1 1 d . . . . .
H6 H 0.700(3) 0.2441(18) 0.3128(15) 0.017(3) Uiso 1 1 d . . . . .
H7 H 0.215(5) 0.111(3) 0.456(3) 0.076(7) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co01 0.00807(4) 0.00976(4) 0.00734(4) 0.00235(3) 0.00260(3) 0.00003(3)
O002 0.01028(14) 0.01220(15) 0.01177(15) 0.00290(12) 0.00331(12) 0.00109(11)
O003 0.01426(16) 0.01215(15) 0.00934(14) 0.00268(12) 0.00117(12) -0.00278(12)
O004 0.01138(15) 0.01399(15) 0.00805(13) 0.00119(11) 0.00290(11) -0.00070(12)
O005 0.01445(17) 0.0222(2) 0.00945(15) 0.00096(14) 0.00298(13) -0.00620(14)
O006 0.01267(16) 0.0228(2) 0.00985(15) 0.00105(14) 0.00398(13) -0.00614(14)
O007 0.0227(2) 0.01393(16) 0.00796(14) 0.00188(12) 0.00369(14) -0.00126(14)
C008 0.01314(18) 0.01080(17) 0.00855(16) 0.00268(14) 0.00275(14) 0.00108(14)
C009 0.00956(17) 0.01157(17) 0.00830(16) 0.00255(13) 0.00279(13) 0.00077(13)
C00A 0.01036(17) 0.01436(19) 0.00950(17) 0.00199(14) 0.00383(14) -0.00080(14)
C00B 0.01251(18) 0.01388(19) 0.00945(17) 0.00243(15) 0.00462(15) -0.00006(15)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co01 O003 2.0384(4) . ?
Co01 O003 2.0384(4) 2_667 ?
Co01 O004 2.1229(4) . ?
Co01 O004 2.1229(4) 2_667 ?
Co01 O002 2.1292(4) . ?
Co01 O002 2.1292(4) 2_667 ?
O002 H1 0.780(16) . ?
O002 H2 0.798(15) . ?
O003 H3 0.775(18) . ?
O003 H4 0.807(16) . ?
O004 C009 1.2587(7) . ?
O005 C008 1.2986(7) . ?
O005 H7 1.05(2) . ?
O006 C009 1.2699(7) . ?
O006 H7 1.38(2) . ?
O007 C008 1.2359(7) . ?
C008 C00B 1.4941(8) . ?
C009 C00A 1.4956(7) . ?
C00A C00B 1.3456(8) . ?
C00A H5 0.950(15) . ?
C00B H6 0.942(13) . ?

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
O003 Co01 O003 180.0 . 2_667 ?
O003 Co01 O004 83.294(18) . . ?
O003 Co01 O004 96.707(18) 2_667 . ?
O003 Co01 O004 96.706(18) . 2_667 ?
O003 Co01 O004 83.294(18) 2_667 2_667 ?
O004 Co01 O004 180.000(10) . 2_667 ?
O003 Co01 O002 88.688(19) . . ?
O003 Co01 O002 91.312(19) 2_667 . ?
O004 Co01 O002 91.464(18) . . ?
O004 Co01 O002 88.536(17) 2_667 . ?
O003 Co01 O002 91.311(19) . 2_667 ?
O003 Co01 O002 88.688(19) 2_667 2_667 ?
O004 Co01 O002 88.536(17) . 2_667 ?
O004 Co01 O002 91.464(18) 2_667 2_667 ?
O002 Co01 O002 180.0 . 2_667 ?
Co01 O002 H1 108.9(12) . . ?
Co01 O002 H2 116.2(10) . . ?
H1 O002 H2 104.2(15) . . ?
Co01 O003 H3 124.5(13) . . ?
Co01 O003 H4 119.2(11) . . ?
H3 O003 H4 110.2(16) . . ?
C009 O004 Co01 127.66(4) . . ?
C008 O005 H7 110.9(13) . . ?
C009 O006 H7 111.0(10) . . ?
O007 C008 O005 121.65(5) . . ?
O007 C008 C00B 118.06(5) . . ?
O005 C008 C00B 120.27(5) . . ?
O004 C009 O006 122.87(5) . . ?
O004 C009 C00A 116.19(5) . . ?
O006 C009 C00A 120.94(5) . . ?
C00B C00A C009 129.78(5) . . ?
C00B C00A H5 117.6(9) . . ?
C009 C00A H5 112.6(9) . . ?
C00A C00B C008 130.28(5) . . ?
C00A C00B H6 116.8(8) . . ?
C008 C00B H6 112.9(8) . . ?

_refine_diff_density_max         0.819
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.087

_shelxl_version_number           2014/6

_shelx_res_file                  
;
TITL mo_cobalt_mal_12_12_0ma_a_a.res in P-1
CELL  0.71073   5.1742   7.2742   9.2053  108.809  105.003   92.409
ZERR    1.000   0.0003   0.0004   0.0005    0.002    0.002    0.003
LATT 1
SFAC C  H  Co O
UNIT 8  14  1  12
REM Old TITL mo_cobalt_mal_12_12_0ma_a.res in P-1
REM SHELXT solution in P-1
REM R1 0.046,  Rweak 0.006,  Alpha 0.038,  Orientation as input
REM Formula found by SHELXT:  C8 Co O12
L.S. 50
ACTA
BOND $H
FMAP 2
PLAN 2
TEMP -183.000
WGHT    0.027100    0.039800
FVAR       1.01106
CO01  3    0.500000    0.500000    1.000000    10.50000    0.00807    0.00976 =
         0.00734    0.00235    0.00260    0.00003
O002  4    0.178182    0.634385    0.897721    11.00000    0.01028    0.01220 =
         0.01177    0.00290    0.00331    0.00109
O003  4    0.747300    0.758613    1.075121    11.00000    0.01426    0.01215 =
         0.00934    0.00268    0.00117   -0.00278
O004  4    0.642120    0.439112    0.794955    11.00000    0.01138    0.01399 =
         0.00805    0.00119    0.00290   -0.00070
O005  4    0.157292    0.037102    0.332402    11.00000    0.01445    0.02224 =
         0.00945    0.00096    0.00298   -0.00620
O006  4    0.295791    0.224381    0.616782    11.00000    0.01267    0.02284 =
         0.00985    0.00105    0.00398   -0.00614
O007  4    0.299124    0.021228    0.122094    11.00000    0.02267    0.01393 =
         0.00796    0.00188    0.00369   -0.00126
C008  1    0.331657    0.087599    0.268196    11.00000    0.01314    0.01080 =
         0.00855    0.00268    0.00275    0.00108
C009  1    0.523445    0.326937    0.654297    11.00000    0.00956    0.01157 =
         0.00830    0.00255    0.00279    0.00077
C00A  1    0.664603    0.321370    0.530525    11.00000    0.01036    0.01436 =
         0.00950    0.00199    0.00383   -0.00080
C00B  1    0.582964    0.225204    0.371245    11.00000    0.01251    0.01388 =
         0.00945    0.00243    0.00462   -0.00006
H1    2    0.177211    0.736611    0.959981    11.00000    0.02989
H2    2    0.029340    0.578853    0.875284    11.00000    0.02510
H3    2    0.823736    0.817866    1.163878    11.00000    0.04225
H4    2    0.717215    0.831156    1.024253    11.00000    0.03290
H5    2    0.833445    0.403777    0.574230    11.00000    0.02631
H6    2    0.700320    0.244139    0.312790    11.00000    0.01663
H7    2    0.215285    0.110964    0.456229    11.00000    0.07558
HKLF 4

REM  mo_cobalt_mal_12_12_0ma_a_a.res in P-1
REM R1 =  0.0269 for    4888 Fo > 4sig(Fo)  and  0.0362 for all    5537 data
REM    125 parameters refined using      0 restraints

END

WGHT      0.0271      0.0395

REM Highest difference peak  0.819,  deepest hole -0.893,  1-sigma level  0.087
Q1    1   0.5881  0.5427  1.0569  11.00000  0.05    0.82
Q2    1   0.5962  0.4962  1.0018  11.00000  0.05    0.73
;
_shelx_res_checksum              46138

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_FeMT
_database_code_depnum_ccdc_archive 'CCDC 1408925'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        'Tetra-aqua-bis(hydrogen maleato)-iron(ii)'
_chemical_name_common            'iron maleate tetrahydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         Fe(H2O)4(C4O4H3)2
_chemical_formula_sum            'C8 H14 Fe O12'
_chemical_formula_weight         358.04

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'
Fe Fe 0.3463 0.8444 '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                   5.2115(2)
_cell_length_b                   7.3307(3)
_cell_length_c                   9.2529(4)
_cell_angle_alpha                109.019(2)
_cell_angle_beta                 105.339(2)
_cell_angle_gamma                92.530(2)
_cell_volume                     318.98(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_F_000             184
_exptl_transmission_factor_min   0.6832
_exptl_transmission_factor_max   0.7479
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    1.248
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30234
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.437
_diffrn_reflns_theta_max         40.022
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3913
_reflns_number_gt                3357
_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 APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_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)+(0.0356P)²+0.0682P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         3913
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0715
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
Fe01 Fe 0.5000 0.5000 0.0000 0.00855(5) Uani 1 2 d S . P . .
O002 O 0.17720(13) 0.63679(10) -0.09859(8) 0.01160(11) Uani 1 1 d . . . . .
O003 O 0.74629(15) 0.76480(11) 0.07585(9) 0.01329(12) Uani 1 1 d . . . . .
O004 O 0.35109(13) 0.56021(10) 0.20507(8) 0.01203(11) Uani 1 1 d . . . . .
O005 O 0.83957(15) 0.96188(12) 0.66623(9) 0.01745(14) Uani 1 1 d . . . . .
O006 O 0.69823(14) 0.77287(12) 0.38291(9) 0.01694(14) Uani 1 1 d . . . . .
O007 O 0.70346(16) 0.97873(11) 0.87655(8) 0.01576(13) Uani 1 1 d . . . . .
C008 C 0.66828(18) 0.91217(13) 0.73082(10) 0.01099(13) Uani 1 1 d . . . . .
C009 C 0.47135(17) 0.67211(13) 0.34583(10) 0.01005(13) Uani 1 1 d . . . . .
C00A C 0.33286(18) 0.67884(14) 0.46937(11) 0.01230(14) Uani 1 1 d . . . . .
C00B C 0.41687(18) 0.77514(13) 0.62823(11) 0.01232(14) Uani 1 1 d . . . . .
H1 H 0.833(4) 0.827(3) 0.162(3) 0.041(6) Uiso 1 1 d . . . . .
H2 H 0.719(4) 0.835(3) 0.023(2) 0.025(4) Uiso 1 1 d . . . . .
H3 H 0.179(4) 0.742(3) -0.038(2) 0.031(5) Uiso 1 1 d . . . . .
H4 H 0.028(4) 0.582(3) -0.125(2) 0.027(4) Uiso 1 1 d . . . . .
H5 H 0.165(4) 0.597(3) 0.427(2) 0.024(4) Uiso 1 1 d . . . . .
H6 H 0.305(3) 0.761(2) 0.6885(18) 0.014(3) Uiso 1 1 d . . . . .
H7 H 0.778(6) 0.893(4) 0.547(4) 0.077(9) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe01 0.00718(7) 0.01020(8) 0.00823(8) 0.00267(6) 0.00299(5) 0.00089(5)
O002 0.0091(2) 0.0122(3) 0.0122(3) 0.0028(2) 0.0029(2) 0.0011(2)
O003 0.0144(3) 0.0128(3) 0.0099(3) 0.0035(2) 0.0006(2) -0.0033(2)
O004 0.0106(2) 0.0148(3) 0.0081(3) 0.0011(2) 0.0025(2) -0.0004(2)
O005 0.0143(3) 0.0234(4) 0.0094(3) 0.0009(3) 0.0026(2) -0.0066(3)
O006 0.0120(3) 0.0246(4) 0.0098(3) 0.0009(3) 0.0037(2) -0.0061(2)
O007 0.0230(3) 0.0140(3) 0.0081(3) 0.0021(2) 0.0039(2) -0.0007(2)
C008 0.0130(3) 0.0107(3) 0.0087(3) 0.0031(3) 0.0026(3) 0.0019(3)
C009 0.0094(3) 0.0118(3) 0.0087(3) 0.0029(3) 0.0031(2) 0.0017(3)
C00A 0.0098(3) 0.0156(4) 0.0101(3) 0.0024(3) 0.0037(3) -0.0005(3)
C00B 0.0125(3) 0.0142(4) 0.0098(3) 0.0026(3) 0.0048(3) 0.0006(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
Fe01 O003 2.0793(7) . ?
Fe01 O003 2.0793(7) 2_665 ?
Fe01 O002 2.1450(7) . ?
Fe01 O002 2.1450(7) 2_665 ?
Fe01 O004 2.1589(7) 2_665 ?
Fe01 O004 2.1590(6) . ?
O002 H3 0.79(2) . ?
O002 H4 0.797(19) . ?
O003 H1 0.78(2) . ?
O003 H2 0.805(19) . ?
O004 C009 1.2603(11) . ?
O005 C008 1.2970(11) . ?
O005 H7 1.01(3) . ?
O006 C009 1.2667(11) . ?
O006 H7 1.42(3) . ?
O007 C008 1.2339(11) . ?
C008 C00B 1.4937(13) . ?
C009 C00A 1.4943(12) . ?
C00A C00B 1.3441(13) . ?
C00A H5 0.947(18) . ?
C00B H6 0.931(16) . ?

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
O003 Fe01 O003 180.0 . 2_665 ?
O003 Fe01 O002 87.38(3) . . ?
O003 Fe01 O002 92.62(3) 2_665 . ?
O003 Fe01 O002 92.62(3) . 2_665 ?
O003 Fe01 O002 87.38(3) 2_665 2_665 ?
O002 Fe01 O002 180.0 . 2_665 ?
O003 Fe01 O004 82.74(3) . 2_665 ?
O003 Fe01 O004 97.26(3) 2_665 2_665 ?
O002 Fe01 O004 93.13(3) . 2_665 ?
O002 Fe01 O004 86.87(3) 2_665 2_665 ?
O003 Fe01 O004 97.26(3) . . ?
O003 Fe01 O004 82.74(3) 2_665 . ?
O002 Fe01 O004 86.87(3) . . ?
O002 Fe01 O004 93.13(3) 2_665 . ?
O004 Fe01 O004 180.0 2_665 . ?
Fe01 O002 H3 110.6(14) . . ?
Fe01 O002 H4 118.0(13) . . ?
H3 O002 H4 106.3(19) . . ?
Fe01 O003 H1 127.8(16) . . ?
Fe01 O003 H2 119.8(13) . . ?
H1 O003 H2 109(2) . . ?
C009 O004 Fe01 126.57(6) . . ?
C008 O005 H7 110.6(17) . . ?
C009 O006 H7 110.5(12) . . ?
O007 C008 O005 121.71(9) . . ?
O007 C008 C00B 118.10(8) . . ?
O005 C008 C00B 120.17(8) . . ?
O004 C009 O006 122.64(8) . . ?
O004 C009 C00A 116.30(8) . . ?
O006 C009 C00A 121.06(8) . . ?
C00B C00A C009 129.67(8) . . ?
C00B C00A H5 117.1(11) . . ?
C009 C00A H5 113.2(11) . . ?
C00A C00B C008 130.31(8) . . ?
C00A C00B H6 118.4(10) . . ?
C008 C00B H6 111.3(9) . . ?

_refine_diff_density_max         1.178
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.103

_shelxl_version_number           2014/6

_shelx_res_file                  
;
TITL mo_FeMal_12_14_0mab_a.res in P-1
CELL  0.71073   5.2115   7.3307   9.2529  109.019  105.339   92.530
ZERR    1.000   0.0002   0.0003   0.0004    0.002    0.002    0.002
LATT 1
SFAC C  H  O  Fe
UNIT 8  14  12  1
REM Old TITL mo_FeMal_12_14_0mab in P-1
REM SHELXT solution in P-1
REM R1 0.053,  Rweak 0.005,  Alpha 0.035,  Orientation as input
REM Formula found by SHELXT:  C8 O12 Fe
L.S. 50
ACTA
BOND $H
FMAP 2
PLAN 3
TEMP -183.000
WGHT    0.035600    0.068200
FVAR       1.01762
FE01  4    0.500000    0.500000    0.000000    10.50000    0.00718    0.01020 =
         0.00823    0.00267    0.00299    0.00089
O002  3    0.177200    0.636786   -0.098587    11.00000    0.00908    0.01223 =
         0.01216    0.00279    0.00288    0.00114
O003  3    0.746291    0.764797    0.075855    11.00000    0.01436    0.01280 =
         0.00994    0.00347    0.00057   -0.00332
O004  3    0.351093    0.560207    0.205075    11.00000    0.01060    0.01479 =
         0.00809    0.00110    0.00252   -0.00043
O005  3    0.839574    0.961876    0.666226    11.00000    0.01433    0.02341 =
         0.00939    0.00092    0.00257   -0.00662
O006  3    0.698232    0.772868    0.382912    11.00000    0.01200    0.02456 =
         0.00976    0.00091    0.00369   -0.00610
O007  3    0.703456    0.978728    0.876550    11.00000    0.02303    0.01400 =
         0.00813    0.00213    0.00389   -0.00073
C008  1    0.668283    0.912174    0.730818    11.00000    0.01298    0.01070 =
         0.00869    0.00307    0.00262    0.00187
C009  1    0.471346    0.672110    0.345834    11.00000    0.00935    0.01183 =
         0.00867    0.00285    0.00310    0.00173
C00A  1    0.332858    0.678843    0.469372    11.00000    0.00975    0.01560 =
         0.01014    0.00237    0.00372   -0.00052
C00B  1    0.416869    0.775142    0.628226    11.00000    0.01254    0.01420 =
         0.00976    0.00259    0.00476    0.00060
H1    2    0.832515    0.826681    0.162402    11.00000    0.04077
H2    2    0.718642    0.834543    0.023470    11.00000    0.02496
H3    2    0.179229    0.742283   -0.037575    11.00000    0.03092
H4    2    0.027614    0.582093   -0.125111    11.00000    0.02682
H5    2    0.164852    0.597341    0.427106    11.00000    0.02405
H6    2    0.305016    0.760875    0.688508    11.00000    0.01384
H7    2    0.778447    0.892672    0.546709    11.00000    0.07739
HKLF 4

REM  mo_FeMal_12_14_0mab_a.res in P-1
REM R1 =  0.0374 for    3357 Fo > 4sig(Fo)  and  0.0494 for all    3913 data
REM    125 parameters refined using      0 restraints

END

WGHT      0.0354      0.0659

REM Highest difference peak  1.178,  deepest hole -0.446,  1-sigma level  0.103
Q1    1   0.4446  0.4580 -0.0775  11.00000  0.05    1.18
Q2    1   0.4012  0.5467 -0.0037  11.00000  0.05    0.94
Q3    1   0.3868  0.7311  0.5535  11.00000  0.05    0.93
;
_shelx_res_checksum              17214

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_MnMT
_database_code_depnum_ccdc_archive 'CCDC 1408926'
_audit_update_record             
;
2015-06-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
'Tetra-aqua-bis(hydrogen maleato)-manganese(ii)'
_chemical_name_common            'manganese maleate tetrahydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         Mn(H2O)4(C4O4H3)2
_chemical_formula_sum            'C8 H14 Mn O12'
_chemical_formula_weight         357.13

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'
Mn Mn 0.3368 0.7283 '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                   5.2823(2)
_cell_length_b                   7.3398(3)
_cell_length_c                   9.3651(3)
_cell_angle_alpha                109.765(2)
_cell_angle_beta                 105.152(2)
_cell_angle_gamma                92.454(2)
_cell_volume                     326.37(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_F_000             183
_exptl_transmission_factor_min   0.6799
_exptl_transmission_factor_max   0.7504
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    1.076
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14510
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.417
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.909
_reflns_number_total             1075
_reflns_number_gt                1012
_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 APEX2 (Bruker, 2011)'
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2010)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2011)'
_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)+(0.0188P)²+0.1699P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         1075
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0421
_refine_ls_wR_factor_gt          0.0411
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
Mn01 Mn 0.5000 0.5000 1.0000 0.01275(11) Uani 1 2 d S . P . .
O002 O 0.8269(2) 0.36186(17) 1.10178(13) 0.0163(2) Uani 1 1 d . . . . .
O003 O 0.65084(19) 0.44009(14) 0.79083(11) 0.0166(2) Uani 1 1 d . . . . .
O004 O 0.7460(2) 0.77361(16) 1.07949(15) 0.0191(2) Uani 1 1 d . . . . .
O005 O 0.1621(2) 0.04001(16) 0.33326(12) 0.0227(3) Uani 1 1 d . . . . .
O006 O 0.2898(2) 0.02409(15) 0.12344(12) 0.0208(2) Uani 1 1 d . . . . .
O007 O 0.3051(2) 0.23071(16) 0.61467(12) 0.0216(3) Uani 1 1 d . . . . .
C008 C 0.3298(3) 0.0885(2) 0.26845(17) 0.0152(3) Uani 1 1 d . . . . .
C009 C 0.5811(3) 0.2222(2) 0.37068(17) 0.0165(3) Uani 1 1 d . . . . .
C00A C 0.6666(3) 0.3181(2) 0.52747(17) 0.0162(3) Uani 1 1 d . . . . .
C00B C 0.5316(3) 0.3291(2) 0.65127(17) 0.0140(3) Uani 1 1 d . . . . .
H1 H 0.722(4) 0.842(3) 1.027(3) 0.040(6) Uiso 1 1 d . . . . .
H2 H 0.840(4) 0.838(3) 1.164(3) 0.038(6) Uiso 1 1 d . . . . .
H3 H 0.980(4) 0.420(3) 1.130(2) 0.034(5) Uiso 1 1 d . . . . .
H4 H 0.825(4) 0.257(3) 1.041(3) 0.036(6) Uiso 1 1 d . . . . .
H5 H 0.224(5) 0.125(4) 0.470(3) 0.084(9) Uiso 1 1 d . . . . .
H6 H 0.690(3) 0.237(2) 0.313(2) 0.020(4) Uiso 1 1 d . . . . .
H7 H 0.833(4) 0.393(3) 0.570(2) 0.023(4) Uiso 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn01 0.01179(16) 0.01409(17) 0.01237(17) 0.00459(13) 0.00408(12) 0.00017(12)
O002 0.0141(6) 0.0159(6) 0.0165(6) 0.0032(5) 0.0042(4) 0.0010(4)
O003 0.0160(5) 0.0189(5) 0.0114(5) 0.0020(4) 0.0034(4) -0.0007(4)
O004 0.0212(6) 0.0187(6) 0.0130(6) 0.0058(5) -0.0006(5) -0.0055(5)
O005 0.0195(6) 0.0292(6) 0.0133(6) 0.0028(5) 0.0030(4) -0.0075(5)
O006 0.0307(6) 0.0176(6) 0.0106(5) 0.0031(4) 0.0037(5) -0.0020(4)
O007 0.0168(5) 0.0303(6) 0.0127(5) 0.0022(5) 0.0049(4) -0.0065(5)
C008 0.0188(7) 0.0128(7) 0.0145(8) 0.0055(6) 0.0044(6) 0.0045(6)
C009 0.0174(7) 0.0179(8) 0.0160(8) 0.0060(6) 0.0081(6) 0.0028(6)
C00A 0.0127(7) 0.0170(8) 0.0168(8) 0.0039(6) 0.0042(6) -0.0010(6)
C00B 0.0143(7) 0.0143(7) 0.0133(7) 0.0052(6) 0.0033(6) 0.0035(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
Mn01 O004 2.1296(11) . ?
Mn01 O004 2.1296(11) 2_667 ?
Mn01 O002 2.2047(10) 2_667 ?
Mn01 O002 2.2047(10) . ?
Mn01 O003 2.2201(9) 2_667 ?
Mn01 O003 2.2201(9) . ?
O002 H3 0.83(2) . ?
O002 H4 0.79(2) . ?
O003 C00B 1.2548(17) . ?
O004 H1 0.81(2) . ?
O004 H2 0.79(2) . ?
O005 C008 1.2961(18) . ?
O005 H5 1.16(3) . ?
O006 C008 1.2327(17) . ?
O007 C00B 1.2706(18) . ?
O007 H5 1.26(3) . ?
C008 C009 1.494(2) . ?
C009 C00A 1.335(2) . ?
C009 H6 0.913(17) . ?
C00A C00B 1.494(2) . ?
C00A H7 0.929(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O004 Mn01 O004 180.0 . 2_667 ?
O004 Mn01 O002 87.23(5) . 2_667 ?
O004 Mn01 O002 92.77(5) 2_667 2_667 ?
O004 Mn01 O002 92.77(5) . . ?
O004 Mn01 O002 87.23(5) 2_667 . ?
O002 Mn01 O002 180.00(4) 2_667 . ?
O004 Mn01 O003 97.30(4) . 2_667 ?
O004 Mn01 O003 82.70(4) 2_667 2_667 ?
O002 Mn01 O003 87.92(4) 2_667 2_667 ?
O002 Mn01 O003 92.08(4) . 2_667 ?
O004 Mn01 O003 82.70(4) . . ?
O004 Mn01 O003 97.30(4) 2_667 . ?
O002 Mn01 O003 92.08(4) 2_667 . ?
O002 Mn01 O003 87.92(4) . . ?
O003 Mn01 O003 180.0 2_667 . ?
Mn01 O002 H3 117.9(14) . . ?
Mn01 O002 H4 110.2(15) . . ?
H3 O002 H4 107(2) . . ?
C00B O003 Mn01 126.27(9) . . ?
Mn01 O004 H1 119.9(15) . . ?
Mn01 O004 H2 130.7(15) . . ?
H1 O004 H2 108(2) . . ?
C008 O005 H5 111.9(13) . . ?
C00B O007 H5 112.0(12) . . ?
O006 C008 O005 121.63(13) . . ?
O006 C008 C009 118.56(13) . . ?
O005 C008 C009 119.79(13) . . ?
C00A C009 C008 130.64(14) . . ?
C00A C009 H6 117.5(10) . . ?
C008 C009 H6 111.8(10) . . ?
C009 C00A C00B 129.85(14) . . ?
C009 C00A H7 117.8(10) . . ?
C00B C00A H7 112.3(10) . . ?
O003 C00B O007 122.22(12) . . ?
O003 C00B C00A 117.03(12) . . ?
O007 C00B C00A 120.75(13) . . ?

_refine_diff_density_max         0.204
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.040

_shelxl_version_number           2014/6

_shelx_res_file                  
;
TITL mo_matrix_0mab_a.res in P-1
CELL  0.71073   5.2823   7.3398   9.3651  109.765  105.152   92.454
ZERR    1.000   0.0002   0.0003   0.0003    0.002    0.002    0.002
LATT 1
SFAC C  H  O  Mn
UNIT 8  14  12  1
REM Old TITL mo_matrix_0mab in P-1
REM SHELXT solution in P-1
REM R1 0.057,  Rweak 0.006,  Alpha 0.081,  Orientation as input
REM Formula found by SHELXT:  C8 O12 Mn
L.S. 50
ACTA
BOND $H
FMAP 2
PLAN 2
TEMP -183.000
WGHT    0.018800    0.169900
FVAR       1.10129
MN01  4    0.500000    0.500000    1.000000    10.50000    0.01179    0.01409 =
         0.01237    0.00459    0.00408    0.00017
O002  3    0.826866    0.361859    1.101776    11.00000    0.01405    0.01587 =
         0.01654    0.00324    0.00421    0.00096
O003  3    0.650844    0.440087    0.790833    11.00000    0.01596    0.01892 =
         0.01135    0.00196    0.00341   -0.00070
O004  3    0.745974    0.773612    1.079492    11.00000    0.02119    0.01875 =
         0.01303    0.00577   -0.00057   -0.00548
O005  3    0.162070    0.040008    0.333265    11.00000    0.01955    0.02921 =
         0.01331    0.00277    0.00297   -0.00752
O006  3    0.289840    0.024089    0.123442    11.00000    0.03070    0.01764 =
         0.01061    0.00313    0.00365   -0.00198
O007  3    0.305068    0.230707    0.614673    11.00000    0.01683    0.03033 =
         0.01267    0.00221    0.00489   -0.00649
C008  1    0.329774    0.088450    0.268445    11.00000    0.01881    0.01284 =
         0.01448    0.00553    0.00443    0.00454
C009  1    0.581138    0.222210    0.370678    11.00000    0.01738    0.01789 =
         0.01601    0.00599    0.00810    0.00276
C00A  1    0.666553    0.318094    0.527470    11.00000    0.01273    0.01699 =
         0.01680    0.00395    0.00422   -0.00097
C00B  1    0.531585    0.329051    0.651266    11.00000    0.01431    0.01428 =
         0.01335    0.00523    0.00332    0.00351
H1    2    0.722250    0.841558    1.026580    11.00000    0.04024
H2    2    0.840424    0.838302    1.164438    11.00000    0.03781
H3    2    0.980425    0.420006    1.130272    11.00000    0.03445
H4    2    0.825413    0.256524    1.041134    11.00000    0.03580
H5    2    0.224250    0.124738    0.469637    11.00000    0.08360
H6    2    0.689750    0.236837    0.312673    11.00000    0.01961
H7    2    0.833008    0.393327    0.569939    11.00000    0.02337
HKLF 4

REM  mo_matrix_0mab_a.res in P-1
REM R1 =  0.0166 for    1012 Fo > 4sig(Fo)  and  0.0185 for all    1075 data
REM    125 parameters refined using      0 restraints

END

WGHT      0.0185      0.1695

REM Highest difference peak  0.204,  deepest hole -0.188,  1-sigma level  0.040
Q1    1   0.5879  0.3244  0.5770  11.00000  0.05    0.20
Q2    1   0.5697  0.2996  0.4427  11.00000  0.05    0.16
;
_shelx_res_checksum              41203

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
