# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_try

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H7 Mg N O7'
_chemical_formula_weight         241.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   4.74600(10)
_cell_length_b                   21.0254(6)
_cell_length_c                   8.6046(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2790(10)
_cell_angle_gamma                90.00
_cell_volume                     858.41(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    120
_cell_measurement_theta_min      3
_cell_measurement_theta_max      30

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_process_details   SADABAS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13772
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.16
_reflns_number_total             1898
_reflns_number_gt                1834
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0497P)²+0.3826P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1898
_refine_ls_number_parameters     173
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0890
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.008

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg1 Mg 0.31050(9) 0.62019(2) 0.68303(5) 0.01555(15) Uani 1 1 d . . .
O1 O 0.0244(2) 0.44267(5) 1.35795(11) 0.0202(2) Uani 1 1 d . . .
O2 O 0.1025(2) 0.64364(5) 0.88719(12) 0.0211(2) Uani 1 1 d . . .
O3 O 0.4726(2) 0.60370(5) 0.46421(11) 0.0189(2) Uani 1 1 d . . .
O4 O 0.4575(3) 0.69726(5) 0.34136(15) 0.0345(3) Uani 1 1 d . . .
O5 O 0.5702(2) 0.54718(5) 0.76938(12) 0.0203(2) Uani 1 1 d . . .
O6 O 0.6156(2) 0.68724(5) 0.74023(13) 0.0223(2) Uani 1 1 d . . .
H6 H 0.564(5) 0.7259(11) 0.771(3) 0.041(6) Uiso 1 1 d . . .
H7 H 0.748(5) 0.6777(11) 0.790(3) 0.042(6) Uiso 1 1 d . . .
O7 O 0.1049(2) 0.69720(6) 0.57859(14) 0.0284(3) Uani 1 1 d . . .
H5 H -0.063(6) 0.7025(12) 0.582(3) 0.059(8) Uiso 1 1 d . . .
H4 H 0.168(6) 0.7093(14) 0.493(3) 0.071(8) Uiso 1 1 d . . .
N1 N -0.1148(2) 0.56215(5) 1.29354(13) 0.0165(2) Uani 1 1 d . . .
H1 H -0.167(4) 0.5451(9) 1.376(2) 0.024(4) Uiso 1 1 d . . .
C1 C 0.1929(3) 0.47117(6) 1.27158(15) 0.0154(3) Uani 1 1 d . . .
C2 C 0.0902(3) 0.53496(6) 1.21032(15) 0.0152(3) Uani 1 1 d . . .
C3 C 0.1770(3) 0.56264(6) 1.07591(15) 0.0163(3) Uani 1 1 d . . .
H3 H 0.322(4) 0.5433(9) 1.020(2) 0.027(5) Uiso 1 1 d . . .
C4 C 0.0450(3) 0.61908(6) 1.01862(15) 0.0161(3) Uani 1 1 d . . .
C5 C 0.5446(3) 0.64208(6) 0.36132(15) 0.0170(3) Uani 1 1 d . . .
C6 C -0.2363(3) 0.61751(6) 1.25042(15) 0.0156(3) Uani 1 1 d . . .
C7 C -0.1637(3) 0.64663(6) 1.11574(16) 0.0181(3) Uani 1 1 d . . .
H2 H -0.250(4) 0.6831(9) 1.086(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
Mg1 0.0161(2) 0.0158(2) 0.0150(2) 0.00244(16) 0.00600(17) 0.00228(15)
O1 0.0196(5) 0.0200(5) 0.0213(5) 0.0046(4) 0.0052(4) -0.0008(4)
O2 0.0250(5) 0.0237(5) 0.0149(5) 0.0042(4) 0.0084(4) 0.0048(4)
O3 0.0219(5) 0.0185(5) 0.0168(5) 0.0026(4) 0.0080(4) 0.0030(4)
O4 0.0452(7) 0.0203(5) 0.0392(7) 0.0104(5) 0.0275(6) 0.0123(5)
O5 0.0188(5) 0.0209(5) 0.0214(5) 0.0045(4) 0.0068(4) 0.0061(4)
O6 0.0199(5) 0.0200(5) 0.0269(5) -0.0029(4) 0.0020(4) 0.0026(4)
O7 0.0252(6) 0.0323(6) 0.0281(6) 0.0122(5) 0.0120(4) 0.0112(4)
N1 0.0177(5) 0.0179(5) 0.0140(5) 0.0033(4) 0.0061(4) 0.0021(4)
C1 0.0168(6) 0.0157(6) 0.0138(6) -0.0002(5) 0.0012(4) 0.0003(5)
C2 0.0142(6) 0.0157(6) 0.0157(6) -0.0003(5) 0.0020(4) 0.0008(4)
C3 0.0157(6) 0.0180(6) 0.0156(6) -0.0010(5) 0.0050(5) 0.0013(5)
C4 0.0170(6) 0.0184(6) 0.0131(6) -0.0003(5) 0.0037(5) -0.0013(5)
C5 0.0176(6) 0.0177(6) 0.0159(6) -0.0002(5) 0.0054(5) 0.0010(5)
C6 0.0159(6) 0.0155(6) 0.0154(6) -0.0012(5) 0.0036(5) 0.0004(4)
C7 0.0211(6) 0.0160(6) 0.0174(6) 0.0017(5) 0.0052(5) 0.0040(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O6 2.0724(12) . ?
Mg1 O3 2.0788(10) . ?
Mg1 O7 2.0839(12) . ?
Mg1 O1 2.0910(11) 3_567 ?
Mg1 O2 2.0931(10) . ?
Mg1 O5 2.0944(10) . ?
O1 C1 1.2559(16) . ?
O1 Mg1 2.0910(11) 3_567 ?
O2 C4 1.2783(16) . ?
O3 C5 1.2511(16) . ?
O4 C5 1.2423(17) . ?
O5 C1 1.2471(16) 3_667 ?
O6 H6 0.89(2) . ?
O6 H7 0.78(3) . ?
O7 H5 0.80(3) . ?
O7 H4 0.84(3) . ?
N1 C6 1.3473(17) . ?
N1 C2 1.3481(16) . ?
N1 H1 0.84(2) . ?
C1 O5 1.2471(16) 3_667 ?
C1 C2 1.5175(18) . ?
C2 C3 1.3664(18) . ?
C3 C4 1.4250(18) . ?
C3 H3 0.94(2) . ?
C4 C7 1.4323(18) . ?
C5 C6 1.5176(17) 1_654 ?
C6 C7 1.3617(19) . ?
C6 C5 1.5176(17) 1_456 ?
C7 H2 0.904(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Mg1 O3 93.31(4) . . ?
O6 Mg1 O7 83.79(5) . . ?
O3 Mg1 O7 85.30(4) . . ?
O6 Mg1 O1 173.98(5) . 3_567 ?
O3 Mg1 O1 92.13(4) . 3_567 ?
O7 Mg1 O1 94.09(5) . 3_567 ?
O6 Mg1 O2 88.88(4) . . ?
O3 Mg1 O2 172.06(4) . . ?
O7 Mg1 O2 87.35(4) . . ?
O1 Mg1 O2 85.38(4) 3_567 . ?
O6 Mg1 O5 90.67(5) . . ?
O3 Mg1 O5 88.42(4) . . ?
O7 Mg1 O5 171.37(5) . . ?
O1 Mg1 O5 92.05(4) 3_567 . ?
O2 Mg1 O5 99.19(4) . . ?
C1 O1 Mg1 133.90(9) . 3_567 ?
C4 O2 Mg1 139.60(9) . . ?
C5 O3 Mg1 130.23(9) . . ?
C1 O5 Mg1 130.83(9) 3_667 . ?
Mg1 O6 H6 119.7(14) . . ?
Mg1 O6 H7 120.3(17) . . ?
H6 O6 H7 107(2) . . ?
Mg1 O7 H5 123.1(19) . . ?
Mg1 O7 H4 116(2) . . ?
H5 O7 H4 111(3) . . ?
C6 N1 C2 121.97(11) . . ?
C6 N1 H1 118.0(12) . . ?
C2 N1 H1 120.0(12) . . ?
O5 C1 O1 127.55(12) 3_667 . ?
O5 C1 C2 117.38(11) 3_667 . ?
O1 C1 C2 115.07(11) . . ?
N1 C2 C3 120.26(12) . . ?
N1 C2 C1 114.85(11) . . ?
C3 C2 C1 124.74(11) . . ?
C2 C3 C4 120.58(12) . . ?
C2 C3 H3 119.1(12) . . ?
C4 C3 H3 120.3(12) . . ?
O2 C4 C3 122.78(12) . . ?
O2 C4 C7 121.13(12) . . ?
C3 C4 C7 116.07(12) . . ?
O4 C5 O3 127.21(12) . . ?
O4 C5 C6 117.49(12) . 1_654 ?
O3 C5 C6 115.29(11) . 1_654 ?
N1 C6 C7 120.53(12) . . ?
N1 C6 C5 114.58(11) . 1_456 ?
C7 C6 C5 124.89(12) . 1_456 ?
C6 C7 C4 120.40(12) . . ?
C6 C7 H2 120.1(12) . . ?
C4 C7 H2 119.5(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.16
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.112
_database_code_depnum_ccdc_archive 'CCDC 987109'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sk_20

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H8 Ca N2 O10'
_chemical_formula_weight         404.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   10.1524(3)
_cell_length_b                   19.9761(6)
_cell_length_c                   7.4902(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.091(2)
_cell_angle_gamma                90.00
_cell_volume                     1515.18(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    120
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27.1

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_process_details   SADABAS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12255
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         27.13
_reflns_number_total             1682
_reflns_number_gt                1391
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART APEX II (Bruker,2010)'
_computing_cell_refinement       'SMART APEX II'
_computing_data_reduction        'SMART APEX II'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia, 1997)'
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0793P)²+2.5233P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0109(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1681
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.1177
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_restrained_S_all      0.883
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.5000 0.08421(3) 0.2500 0.0235(2) Uani 1 2 d S . .
C1 C 0.2479(2) -0.10051(10) 0.2303(3) 0.0259(5) Uani 1 1 d . . .
C2 C 0.1452(2) -0.07855(10) 0.1176(3) 0.0288(5) Uani 1 1 d . . .
H2 H 0.1343 -0.0331 0.0939 0.035 Uiso 1 1 calc R . .
C3 C 0.0565(2) -0.12548(11) 0.0379(3) 0.0269(5) Uani 1 1 d . . .
C4 C 0.0799(2) -0.19403(10) 0.0694(3) 0.0249(4) Uani 1 1 d . . .
H4 H 0.0248 -0.2260 0.0134 0.030 Uiso 1 1 calc R . .
C5 C 0.1844(2) -0.21321(10) 0.1830(3) 0.0239(4) Uani 1 1 d . . .
C6 C 0.3471(2) -0.05660(11) 0.3361(3) 0.0289(5) Uani 1 1 d . . .
C7 C 0.7168(2) 0.21491(10) 0.2362(3) 0.0261(5) Uani 1 1 d . . .
N1 N 0.26390(17) -0.16653(8) 0.2599(2) 0.0255(4) Uani 1 1 d . . .
H1 H 0.3287 -0.1794 0.3320 0.031 Uiso 1 1 calc R . .
O1 O 0.34398(17) 0.00392(8) 0.2990(3) 0.0394(4) Uani 1 1 d . . .
O2 O 0.42135(18) -0.08697(8) 0.4496(2) 0.0383(4) Uani 1 1 d . . .
O3 O 0.63960(16) 0.17128(8) 0.1770(2) 0.0376(4) Uani 1 1 d . . .
O4 O 0.81923(17) 0.20794(8) 0.3366(2) 0.0390(4) Uani 1 1 d . . .
O5 O -0.04744(16) -0.10353(8) -0.0610(2) 0.0359(4) Uani 1 1 d . . .
H5 H -0.0494 -0.0625 -0.0573 0.054 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ca1 0.0248(3) 0.0131(3) 0.0311(4) 0.000 -0.0079(2) 0.000
C1 0.0298(11) 0.0210(10) 0.0265(11) 0.0018(8) -0.0012(8) -0.0046(8)
C2 0.0323(11) 0.0204(10) 0.0327(12) 0.0039(8) -0.0049(9) -0.0036(8)
C3 0.0280(11) 0.0258(10) 0.0263(11) 0.0020(8) -0.0026(8) -0.0021(8)
C4 0.0232(10) 0.0220(10) 0.0289(11) -0.0007(8) -0.0014(8) -0.0048(8)
C5 0.0253(10) 0.0192(9) 0.0271(10) 0.0009(8) 0.0015(8) -0.0031(8)
C6 0.0293(11) 0.0248(11) 0.0317(11) -0.0004(9) -0.0036(9) -0.0057(8)
C7 0.0275(11) 0.0226(10) 0.0282(11) 0.0013(8) 0.0025(8) 0.0003(8)
N1 0.0273(9) 0.0208(9) 0.0274(9) 0.0019(7) -0.0056(7) -0.0026(7)
O1 0.0411(10) 0.0228(8) 0.0528(11) 0.0036(7) -0.0078(8) -0.0093(7)
O2 0.0450(10) 0.0314(9) 0.0357(9) 0.0003(7) -0.0159(8) -0.0055(7)
O3 0.0353(9) 0.0220(8) 0.0543(11) 0.0024(7) -0.0046(8) -0.0090(6)
O4 0.0401(10) 0.0268(8) 0.0476(10) 0.0031(7) -0.0146(8) 0.0017(7)
O5 0.0341(9) 0.0256(8) 0.0454(10) 0.0035(7) -0.0154(7) 0.0007(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
Ca1 O1 2.3020(16) . ?
Ca1 O1 2.3020(16) 2_655 ?
Ca1 O3 2.3330(16) . ?
Ca1 O3 2.3330(16) 2_655 ?
Ca1 O2 2.3340(16) 6 ?
Ca1 O2 2.3340(16) 5_656 ?
C1 N1 1.345(3) . ?
C1 C2 1.366(3) . ?
C1 C6 1.516(3) . ?
C2 C3 1.404(3) . ?
C2 H2 0.9300 . ?
C3 O5 1.320(3) . ?
C3 C4 1.407(3) . ?
C4 C5 1.366(3) . ?
C4 H4 0.9300 . ?
C5 N1 1.336(3) . ?
C5 C7 1.520(3) 3_445 ?
C6 O1 1.240(3) . ?
C6 O2 1.252(3) . ?
C7 O3 1.233(3) . ?
C7 O4 1.247(3) . ?
C7 C5 1.520(3) 3 ?
N1 H1 0.8600 . ?
O2 Ca1 2.3340(16) 5_656 ?
O5 H5 0.8200 . ?

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 Ca1 O1 91.66(9) . 2_655 ?
O1 Ca1 O3 173.31(6) . . ?
O1 Ca1 O3 92.62(6) 2_655 . ?
O1 Ca1 O3 92.62(6) . 2_655 ?
O1 Ca1 O3 173.31(6) 2_655 2_655 ?
O3 Ca1 O3 83.60(9) . 2_655 ?
O1 Ca1 O2 88.75(6) . 6 ?
O1 Ca1 O2 93.14(6) 2_655 6 ?
O3 Ca1 O2 85.89(6) . 6 ?
O3 Ca1 O2 92.09(6) 2_655 6 ?
O1 Ca1 O2 93.14(6) . 5_656 ?
O1 Ca1 O2 88.75(6) 2_655 5_656 ?
O3 Ca1 O2 92.09(6) . 5_656 ?
O3 Ca1 O2 85.89(6) 2_655 5_656 ?
O2 Ca1 O2 177.29(8) 6 5_656 ?
N1 C1 C2 119.62(19) . . ?
N1 C1 C6 114.44(18) . . ?
C2 C1 C6 125.90(19) . . ?
C1 C2 C3 119.12(19) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
O5 C3 C4 122.45(19) . . ?
O5 C3 C2 118.7(2) . . ?
C4 C3 C2 118.87(19) . . ?
C5 C4 C3 119.48(19) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 119.39(19) . . ?
N1 C5 C7 115.70(18) . 3_445 ?
C4 C5 C7 124.88(18) . 3_445 ?
O1 C6 O2 129.0(2) . . ?
O1 C6 C1 116.21(19) . . ?
O2 C6 C1 114.81(18) . . ?
O3 C7 O4 128.3(2) . . ?
O3 C7 C5 116.99(19) . 3 ?
O4 C7 C5 114.76(18) . 3 ?
C5 N1 C1 123.44(18) . . ?
C5 N1 H1 118.3 . . ?
C1 N1 H1 118.3 . . ?
C6 O1 Ca1 135.05(16) . . ?
C6 O2 Ca1 142.31(16) . 5_656 ?
C7 O3 Ca1 145.46(16) . . ?
C3 O5 H5 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.13
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 987110'
