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

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

data_fx3-47e_a
_database_code_depnum_ccdc_archive 'CCDC 1426301'
_audit_update_record             
;
2015-09-22 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 Mg O6'
_chemical_formula_weight         250.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Mg Mg 0.0585 0.0440
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   11.3400(6)
_cell_length_b                   6.6324(3)
_cell_length_c                   7.1986(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.313(3)
_cell_angle_gamma                90
_cell_volume                     528.96(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6120
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      40.31

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.224
_shelx_estimated_absorpt_T_min   0.957
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            9473
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.904
_diffrn_reflns_theta_max         40.307
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2553
_reflns_number_gt                2247
_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 APEX 2'
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_structure_solution    'Bruker SHELXT 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen atoms
 were placed geometrically on the carbon atoms constrained and
 refined using a riding model. On the water they were found in the
 difference map and allow to refine freely. Due to the disorder of
 the ligand geometical and displacement parameter restraints were
 used: SADI; SAME; and EADP. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²+0.4274P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrinsic phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2553
_refine_ls_number_parameters     108
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1133
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_restrained_S_all      1.234
_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
Mg1 Mg 0.5000 0.0000 0.5000 0.00742(11) Uani 1 2 d S . P . .
O1W O 0.58774(8) 0.27659(13) 0.51789(12) 0.01099(15) Uani 1 1 d . . . . .
H1WA H 0.553(2) 0.345(4) 0.427(4) 0.032(6) Uiso 1 1 d . . . . .
H1WB H 0.596(2) 0.351(4) 0.610(4) 0.038(7) Uiso 1 1 d . . . . .
O1 O 0.36023(7) 0.11333(13) 0.29573(12) 0.01069(15) Uani 1 1 d . . . . .
O2 O 0.41409(7) 0.41951(12) 0.21593(11) 0.00926(15) Uani 1 1 d . . . . .
C1 C 0.33478(9) 0.28358(16) 0.22343(14) 0.00821(17) Uani 1 1 d . . . . .
C2 C 0.20533(10) 0.33241(19) 0.14673(18) 0.0145(2) Uani 1 1 d D . . . .
H2A H 0.1494 0.2254 0.1453 0.017 Uiso 0.5 1 calc R U P A 2
C3 C 0.1142(2) 0.2002(4) 0.1325(4) 0.0141(4) Uani 0.5 1 d D . P B -1
H3A H 0.1319 0.0655 0.1738 0.017 Uiso 0.5 1 calc R U P B -1
C4 C -0.0049(2) 0.2536(4) 0.0594(4) 0.0162(4) Uani 0.5 1 d D . P B -1
H4A H -0.0671 0.1572 0.0571 0.019 Uiso 0.5 1 calc R U P B -1
C5 C -0.0345(4) 0.4496(7) -0.0114(7) 0.0157(6) Uani 0.5 1 d D . P B -1
C6 C 0.0576(3) 0.5882(7) -0.0060(8) 0.0188(7) Uani 0.5 1 d D . P B -1
H6A H 0.0388 0.7209 -0.0529 0.023 Uiso 0.5 1 calc R U P B -1
C7 C 0.1783(6) 0.5347(10) 0.0681(14) 0.0158(6) Uani 0.5 1 d D . P B -1
H7A H 0.2415 0.6285 0.0671 0.019 Uiso 0.5 1 calc R U P B -1
C8 C -0.1613(6) 0.4990(10) -0.0831(13) 0.0158(6) Uani 0.5 1 d D . P . .
H8A H -0.2175 0.3929 -0.0820 0.019 Uiso 0.5 1 calc R U P B .


_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 O1 2.0604(8) . ?
Mg1 O1 2.0604(8) 3_656 ?
Mg1 O2 2.0727(8) 4_566 ?
Mg1 O2 2.0727(8) 2_645 ?
Mg1 O1W 2.0778(8) . ?
Mg1 O1W 2.0778(8) 3_656 ?
O1W H1WA 0.83(2) . ?
O1W H1WB 0.81(3) . ?
O1 C1 1.2511(13) . ?
O2 C1 1.2827(13) . ?
O2 Mg1 2.0727(8) 2_655 ?
C1 C2 1.4896(15) . ?
C2 C8 1.270(7) 3_565 ?
C2 C3 1.342(3) . ?
C2 C7 1.463(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.386(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.410(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.386(5) . ?
C5 C8 1.458(8) . ?
C6 C7 1.405(8) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C2 1.270(7) 3_565 ?
C8 H8A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg1 O1 180.0 . 3_656 ?
O1 Mg1 O2 91.62(3) . 4_566 ?
O1 Mg1 O2 88.38(3) 3_656 4_566 ?
O1 Mg1 O2 88.38(3) . 2_645 ?
O1 Mg1 O2 91.62(3) 3_656 2_645 ?
O2 Mg1 O2 180.0 4_566 2_645 ?
O1 Mg1 O1W 90.43(3) . . ?
O1 Mg1 O1W 89.57(3) 3_656 . ?
O2 Mg1 O1W 91.24(3) 4_566 . ?
O2 Mg1 O1W 88.76(3) 2_645 . ?
O1 Mg1 O1W 89.57(3) . 3_656 ?
O1 Mg1 O1W 90.43(3) 3_656 3_656 ?
O2 Mg1 O1W 88.76(3) 4_566 3_656 ?
O2 Mg1 O1W 91.24(3) 2_645 3_656 ?
O1W Mg1 O1W 180.0 . 3_656 ?
Mg1 O1W H1WA 106.9(16) . . ?
Mg1 O1W H1WB 123.5(18) . . ?
H1WA O1W H1WB 105(2) . . ?
C1 O1 Mg1 134.45(7) . . ?
C1 O2 Mg1 131.19(7) . 2_655 ?
O1 C1 O2 123.38(10) . . ?
O1 C1 C2 118.17(10) . . ?
O2 C1 C2 118.43(10) . . ?
C8 C2 C3 108.1(3) 3_565 . ?
C8 C2 C7 11.2(4) 3_565 . ?
C3 C2 C7 118.4(3) . . ?
C8 C2 C1 127.3(3) 3_565 . ?
C3 C2 C1 124.62(14) . . ?
C7 C2 C1 116.8(3) . . ?
C8 C2 H2A 116.4 3_565 . ?
C1 C2 H2A 116.4 . . ?
C2 C3 C4 122.3(2) . . ?
C2 C3 H3A 118.9 . . ?
C4 C3 H3A 118.9 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C6 C5 C4 118.8(2) . . ?
C6 C5 C8 122.8(3) . . ?
C4 C5 C8 118.4(3) . . ?
C5 C6 C7 120.7(3) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C6 C7 C2 119.0(4) . . ?
C6 C7 H7A 120.5 . . ?
C2 C7 H7A 120.5 . . ?
C2 C8 C5 127.4(4) 3_565 . ?
C2 C8 H8A 116.3 3_565 . ?
C5 C8 H8A 116.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O2 0.83(2) 2.00(2) 2.7704(12) 155(2) .
O1W H1WB O2 0.81(3) 1.99(3) 2.7842(12) 164(2) 3_666

_refine_diff_density_max         0.538
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_fx3-36g_a
_database_code_depnum_ccdc_archive 'CCDC 1426302'
_audit_update_record             
;
2015-09-22 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H8 Ca O5'
_chemical_formula_weight         248.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Ca Ca 0.2552 0.3638
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   11.6947(4)
_cell_length_b                   6.8463(3)
_cell_length_c                   12.2702(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.4060(16)
_cell_angle_gamma                90
_cell_volume                     982.39(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9927
_cell_measurement_theta_min      3.71
_cell_measurement_theta_max      40.23

_exptl_crystal_description       tablet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_F_000             512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.803
_shelx_estimated_absorpt_T_min   0.795
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            17010
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.621
_diffrn_reflns_theta_max         42.502
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4757
_reflns_number_gt                4346
_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 APEX 2'
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen atoms
 were placed geometrically on the carbon atoms and constrained, on
 the 25% water they were found in the difference map and restrained
 and refined using a riding model. On the 75% water they were found
 in the difference map restrained and allow to refine freely.
 Displacement parameter restraints were use to model C2' which was
 prolate 7.1 before the restraints were allowed.
;
_vrf_PLAT430_fx3-36g_a           
;
PROBLEM: Short Inter D...A Contact  O3     ..  O4      2.78 Ang.  
RESPONSE: these atoms form 2 mu-2 bridges between two Ca atoms, the
 bridges are opposite each other
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0406P)²+0.2786P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrinsic phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4757
_refine_ls_number_parameters     241
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.046
_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
Ca1 Ca 0.93035(2) 0.20412(2) 0.29057(2) 0.00831(4) Uani 1 1 d D . . . .
O1 O 0.80112(5) 0.21098(11) 0.43587(5) 0.02041(13) Uani 1 1 d . . . . .
O2 O 0.86512(5) 0.32299(10) 0.60238(5) 0.01757(11) Uani 1 1 d . . . . .
C1 C 0.78777(6) 0.27613(11) 0.53453(6) 0.01239(12) Uani 1 1 d . . . . .
C2 C 0.6703(5) 0.3030(9) 0.5723(4) 0.0125(5) Uani 0.7270(19) 1 d . . P A 1
C3 C 0.64554(8) 0.40252(15) 0.67110(8) 0.01196(17) Uani 0.7270(19) 1 d . . P A
1
H3A H 0.7065 0.4486 0.7158 0.014 Uiso 0.7270(19) 1 calc R U P A 1
C4 C 0.53735(8) 0.43207(15) 0.70192(9) 0.01287(18) Uani 0.7270(19) 1 d . . P A
1
H4A H 0.5197 0.5006 0.7670 0.015 Uiso 0.7270(19) 1 calc R U P A 1
C5 C 0.45202(9) 0.35794(18) 0.63436(13) 0.0122(2) Uani 0.7270(19) 1 d . . P A 1
C6 C 0.47705(9) 0.25836(18) 0.53433(13) 0.01272(19) Uani 0.727(2) 1 d . . P A 1
H6A H 0.4160 0.2108 0.4903 0.015 Uiso 0.7270(19) 1 calc R U P A 1
C7 C 0.58495(10) 0.2315(2) 0.50216(12) 0.0120(2) Uani 0.7270(19) 1 d . . P A 1
H7A H 0.6027 0.1677 0.4357 0.014 Uiso 0.7270(19) 1 calc R U P A 1
C8 C 0.33840(11) 0.38725(19) 0.67223(14) 0.0142(2) Uani 0.7270(19) 1 d . U P A
1
H8A H 0.3222 0.4968 0.7171 0.017 Uiso 0.7270(19) 1 calc R U P A 1
C9 C 0.2565(3) 0.2672(3) 0.6466(3) 0.0132(4) Uani 0.7270(19) 1 d . U P A 1
H9A H 0.2697 0.1632 0.5970 0.016 Uiso 0.7270(19) 1 calc R U P A 1
C10 C 0.14607(6) 0.29367(10) 0.69411(6) 0.01098(11) Uani 1 1 d . U . . .
O3 O 0.10715(5) 0.45654(8) 0.72391(6) 0.01635(11) Uani 1 1 d . . . . .
O4 O 0.09098(5) 0.13788(8) 0.70309(5) 0.01263(10) Uani 1 1 d . . . . .
C2' C 0.2641(8) 0.3093(8) 0.6518(8) 0.0130(9) Uani 0.2730(19) 1 d . U P A 2
C3' C 0.2892(2) 0.2088(4) 0.5518(3) 0.0153(5) Uani 0.2730(19) 1 d . U P A 2
H3'A H 0.2302 0.1417 0.5136 0.018 Uiso 0.2730(19) 1 calc R U P A 2
C4' C 0.3955(3) 0.2099(4) 0.5128(3) 0.0158(5) Uani 0.2730(19) 1 d . . P A 2
H4'A H 0.4134 0.1525 0.4445 0.019 Uiso 0.2730(19) 1 calc R U P A 2
C5' C 0.4789(2) 0.2994(5) 0.5774(3) 0.0121(5) Uani 0.2730(19) 1 d . . P A 2
C6' C 0.4530(3) 0.3961(6) 0.6754(4) 0.0179(6) Uani 0.2730(19) 1 d . . P A 2
H6'A H 0.5130 0.4563 0.7157 0.021 Uiso 0.2730(19) 1 calc R U P A 2
C7' C 0.3444(3) 0.4055(6) 0.7141(4) 0.0177(7) Uani 0.2730(19) 1 d . U P A 2
H7'A H 0.3256 0.4734 0.7791 0.021 Uiso 0.2730(19) 1 calc R U P A 2
C8' C 0.5921(3) 0.2773(6) 0.5341(4) 0.0139(6) Uani 0.2730(19) 1 d . . P A 2
H8'A H 0.5989 0.2333 0.4610 0.017 Uiso 0.2730(19) 1 calc R U P A 2
C9' C 0.6816(16) 0.312(3) 0.5856(14) 0.027(3) Uani 0.2730(19) 1 d . . P A 2
H9'A H 0.6789 0.3607 0.6579 0.033 Uiso 0.2730(19) 1 calc R U P A 2
O1W O 1.04115(8) 0.29336(18) 0.44896(8) 0.0210(2) Uani 0.7270(19) 1 d D . P A 1
H1WA H 1.0026(16) 0.302(3) 0.5072(14) 0.036(6) Uiso 0.7270(19) 1 d D . P A 1
H1WB H 1.0731(19) 0.405(3) 0.4447(17) 0.048(7) Uiso 0.7270(19) 1 d D . P A 1
O1W' O 1.04018(19) 0.1774(4) 0.4580(2) 0.0178(5) Uani 0.2730(19) 1 d D . P A 2
H1WC H 1.056(4) 0.060(3) 0.475(3) 0.027 Uiso 0.2730(19) 1 d D U P A 2
H1WD H 1.1078(19) 0.222(7) 0.451(2) 0.027 Uiso 0.2730(19) 1 d D U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.3458(6) . ?
Ca1 O4 2.3560(6) 3_656 ?
Ca1 O3 2.3707(6) 3_666 ?
Ca1 O1W 2.4071(10) . ?
Ca1 O1W' 2.422(2) . ?
Ca1 O4 2.4248(6) 4_665 ?
Ca1 O2 2.4338(6) 4_565 ?
Ca1 O3 2.4855(6) 4_665 ?
Ca1 C10 2.7943(7) 4_665 ?
Ca1 Ca1 3.92252(19) 2_745 ?
Ca1 Ca1 3.92254(18) 2_755 ?
O1 C1 1.3006(10) . ?
O2 C1 1.2663(10) . ?
O2 Ca1 2.4338(6) 4_566 ?
C1 C9' 1.416(18) . ?
C1 C2 1.464(5) . ?
C2 C7 1.402(6) . ?
C2 C3 1.422(4) . ?
C3 C4 1.3386(13) . ?
C3 H3A 0.9500 . ?
C4 C5 1.3888(17) . ?
C4 H4A 0.9500 . ?
C5 C8 1.4250(16) . ?
C5 C6 1.436(2) . ?
C6 C7 1.3374(16) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.299(3) . ?
C8 H8A 0.9500 . ?
C9 C10 1.432(3) . ?
C9 H9A 0.9500 . ?
C10 O4 1.2514(8) . ?
C10 O3 1.2596(9) . ?
C10 C2' 1.481(9) . ?
C10 Ca1 2.7943(7) 4_466 ?
O3 Ca1 2.3707(6) 3_666 ?
O3 Ca1 2.4856(6) 4_466 ?
O4 Ca1 2.3560(6) 3_656 ?
O4 Ca1 2.4248(6) 4_466 ?
C2' C7' 1.375(9) . ?
C2' C3' 1.439(10) . ?
C3' C4' 1.335(4) . ?
C3' H3'A 0.9500 . ?
C4' C5' 1.394(5) . ?
C4' H4'A 0.9500 . ?
C5' C6' 1.408(6) . ?
C5' C8' 1.438(4) . ?
C6' C7' 1.360(5) . ?
C6' H6'A 0.9500 . ?
C7' H7'A 0.9500 . ?
C8' C9' 1.240(18) . ?
C8' H8'A 0.9500 . ?
C9' H9'A 0.9500 . ?
O1W H1WA 0.850(16) . ?
O1W H1WB 0.849(16) . ?
O1W' H1WC 0.852(17) . ?
O1W' H1WD 0.854(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
O1 Ca1 O4 85.75(2) . 3_656 ?
O1 Ca1 O3 85.27(2) . 3_666 ?
O4 Ca1 O3 163.11(2) 3_656 3_666 ?
O1 Ca1 O1W 74.18(3) . . ?
O4 Ca1 O1W 106.38(3) 3_656 . ?
O3 Ca1 O1W 84.84(3) 3_666 . ?
O1 Ca1 O1W' 72.40(6) . . ?
O4 Ca1 O1W' 87.27(7) 3_656 . ?
O3 Ca1 O1W' 103.55(7) 3_666 . ?
O1 Ca1 O4 146.39(2) . 4_665 ?
O4 Ca1 O4 122.715(16) 3_656 4_665 ?
O3 Ca1 O4 70.919(19) 3_666 4_665 ?
O1W Ca1 O4 80.20(3) . 4_665 ?
O1W' Ca1 O4 90.07(6) . 4_665 ?
O1 Ca1 O2 121.56(2) . 4_565 ?
O4 Ca1 O2 85.59(2) 3_656 4_565 ?
O3 Ca1 O2 86.97(2) 3_666 4_565 ?
O1W Ca1 O2 161.57(3) . 4_565 ?
O1W' Ca1 O2 163.68(6) . 4_565 ?
O4 Ca1 O2 81.52(2) 4_665 4_565 ?
O1 Ca1 O3 143.21(2) . 4_665 ?
O4 Ca1 O3 70.096(19) 3_656 4_665 ?
O3 Ca1 O3 124.254(16) 3_666 4_665 ?
O1W Ca1 O3 86.20(3) . 4_665 ?
O1W' Ca1 O3 78.94(6) . 4_665 ?
O4 Ca1 O3 53.336(19) 4_665 4_665 ?
O2 Ca1 O3 84.83(2) 4_565 4_665 ?
O1 Ca1 C10 155.54(2) . 4_665 ?
O4 Ca1 C10 96.629(19) 3_656 4_665 ?
O3 Ca1 C10 97.47(2) 3_666 4_665 ?
O1W Ca1 C10 81.84(3) . 4_665 ?
O1W' Ca1 C10 83.37(6) . 4_665 ?
O4 Ca1 C10 26.554(19) 4_665 4_665 ?
O2 Ca1 C10 82.90(2) 4_565 4_665 ?
O3 Ca1 C10 26.792(18) 4_665 4_665 ?
O1 Ca1 Ca1 118.772(19) . 2_745 ?
O4 Ca1 Ca1 35.446(13) 3_656 2_745 ?
O3 Ca1 Ca1 155.942(16) 3_666 2_745 ?
O1W Ca1 Ca1 101.78(3) . 2_745 ?
O1W' Ca1 Ca1 86.02(6) . 2_745 ?
O4 Ca1 Ca1 87.277(14) 4_665 2_745 ?
O2 Ca1 Ca1 79.665(17) 4_565 2_745 ?
O3 Ca1 Ca1 35.147(13) 4_665 2_745 ?
C10 Ca1 Ca1 61.273(14) 4_665 2_745 ?
O1 Ca1 Ca1 116.513(18) . 2_755 ?
O4 Ca1 Ca1 156.914(15) 3_656 2_755 ?
O3 Ca1 Ca1 37.126(14) 3_666 2_755 ?
O1W Ca1 Ca1 76.19(3) . 2_755 ?
O1W' Ca1 Ca1 93.58(7) . 2_755 ?
O4 Ca1 Ca1 34.298(13) 4_665 2_755 ?
O2 Ca1 Ca1 87.348(17) 4_565 2_755 ?
O3 Ca1 Ca1 87.404(14) 4_665 2_755 ?
C10 Ca1 Ca1 60.654(14) 4_665 2_755 ?
Ca1 Ca1 Ca1 121.545(7) 2_745 2_755 ?
C1 O1 Ca1 142.80(5) . . ?
C1 O2 Ca1 145.29(5) . 4_566 ?
O2 C1 O1 127.51(7) . . ?
O2 C1 C9' 106.9(7) . . ?
O1 C1 C9' 125.6(7) . . ?
O2 C1 C2 115.3(2) . . ?
O1 C1 C2 117.2(2) . . ?
C7 C2 C3 122.8(4) . . ?
C7 C2 C1 115.3(3) . . ?
C3 C2 C1 121.8(4) . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 H3A 119.6 . . ?
C3 C4 C5 116.92(10) . . ?
C3 C4 H4A 121.5 . . ?
C5 C4 H4A 121.5 . . ?
C4 C5 C8 114.94(13) . . ?
C4 C5 C6 122.26(10) . . ?
C8 C5 C6 122.80(12) . . ?
C7 C6 C5 121.06(12) . . ?
C7 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C6 C7 C2 116.1(2) . . ?
C6 C7 H7A 121.9 . . ?
C2 C7 H7A 121.9 . . ?
C9 C8 C5 121.31(18) . . ?
C9 C8 H8A 119.3 . . ?
C5 C8 H8A 119.3 . . ?
C8 C9 C10 119.1(2) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
O4 C10 O3 122.79(6) . . ?
O4 C10 C9 113.23(10) . . ?
O3 C10 C9 123.98(10) . . ?
O4 C10 C2' 125.0(2) . . ?
O3 C10 C2' 112.2(2) . . ?
O4 C10 Ca1 60.02(4) . 4_466 ?
O3 C10 Ca1 62.81(4) . 4_466 ?
C9 C10 Ca1 172.99(10) . 4_466 ?
C2' C10 Ca1 173.7(3) . 4_466 ?
C10 O3 Ca1 155.89(5) . 3_666 ?
C10 O3 Ca1 90.40(4) . 4_466 ?
Ca1 O3 Ca1 107.73(2) 3_666 4_466 ?
C10 O4 Ca1 154.78(5) . 3_656 ?
C10 O4 Ca1 93.42(4) . 4_466 ?
Ca1 O4 Ca1 110.26(2) 3_656 4_466 ?
C7' C2' C3' 124.0(7) . . ?
C7' C2' C10 118.3(7) . . ?
C3' C2' C10 117.4(6) . . ?
C4' C3' C2' 120.0(4) . . ?
C4' C3' H3'A 120.0 . . ?
C2' C3' H3'A 120.0 . . ?
C3' C4' C5' 116.6(3) . . ?
C3' C4' H4'A 121.7 . . ?
C5' C4' H4'A 121.7 . . ?
C4' C5' C6' 122.6(3) . . ?
C4' C5' C8' 112.7(3) . . ?
C6' C5' C8' 124.7(3) . . ?
C7' C6' C5' 121.8(4) . . ?
C7' C6' H6'A 119.1 . . ?
C5' C6' H6'A 119.1 . . ?
C6' C7' C2' 114.8(5) . . ?
C6' C7' H7'A 122.6 . . ?
C2' C7' H7'A 122.6 . . ?
C9' C8' C5' 124.6(9) . . ?
C9' C8' H8'A 117.7 . . ?
C5' C8' H8'A 117.7 . . ?
C8' C9' C1 118.8(12) . . ?
C8' C9' H9'A 120.6 . . ?
C1 C9' H9'A 120.6 . . ?
Ca1 O1W H1WA 114.3(13) . . ?
Ca1 O1W H1WB 114.3(14) . . ?
H1WA O1W H1WB 103(2) . . ?
Ca1 O1W' H1WC 113.6(17) . . ?
Ca1 O1W' H1WD 112.3(17) . . ?
H1WC O1W' H1WD 99(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O2 0.850(16) 1.999(17) 2.8067(12) 158.4(19) .
O1W H1WB O2 0.849(16) 2.084(16) 2.9166(13) 166.6(19) 3_766

_refine_diff_density_max         0.769
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.066

