# Electronic SUpplementary MAterial for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Qiang Xu'
_publ_contact_author_email       Q.XU@AIST.GO.JP

_publ_section_title              
;
Observation of helical water chains reversibly inlayed
in magnesium imidazole-4,5-dicarboxylate
;
loop_
_publ_author_name
'Qiang Xu.'
'Miao Du.'
'Nobuhiko Takeichi'
'Rui-Qin Zhong.'
'Ru-Qiang Zou.'

# Attachment '080411 1.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 655557'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H9 Mg N2 O7.50'
_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   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                   13.936(3)
_cell_length_b                   11.642(2)
_cell_length_c                   12.090(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.27(3)
_cell_angle_gamma                90.00
_cell_volume                     1862.4(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1423
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.40

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7781
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_special_details           
;
Refinement using reflections with F² > -3.0 sigma(F²).
The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are
based on F, with F set to zero for negative F. The threshold expression of
F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7224
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         25.19
_reflns_number_total             1676
_reflns_number_gt                1560
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rigaku RAXIS-RAPID'
_computing_cell_refinement       'Rigaku RAXIS-RAPID'
_computing_data_reduction        'Rigaku RAXIS-RAPID'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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)+(0.0542P)²+1.4437P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1676
_refine_ls_number_parameters     141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0866
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
Mg1 Mg 0.26351(4) 0.74829(4) 0.22054(4) 0.02040(17) Uani 1 1 d . . .
C1 C 0.38579(10) 0.50113(12) 0.14362(12) 0.0182(3) Uani 1 1 d . . .
C2 C 0.33257(10) 0.45125(12) 0.21018(12) 0.0174(3) Uani 1 1 d . . .
C3 C 0.38635(13) 0.31335(13) 0.12683(15) 0.0293(4) Uani 1 1 d . . .
H3 H 0.3992 0.2405 0.1032 0.035 Uiso 1 1 calc R . .
C4 C 0.41161(10) 0.62028(12) 0.11776(12) 0.0191(3) Uani 1 1 d . . .
C5 C 0.28097(10) 0.49435(12) 0.29396(12) 0.0168(3) Uani 1 1 d . . .
N1 N 0.41924(10) 0.41095(11) 0.09298(12) 0.0256(3) Uani 1 1 d . . .
H1A H 0.4571 0.4129 0.0450 0.031 Uiso 1 1 d R . .
N2 N 0.33351(9) 0.33362(11) 0.19790(11) 0.0232(3) Uani 1 1 d . . .
O1 O 0.47566(9) 0.62959(10) 0.06509(10) 0.0305(3) Uani 1 1 d . . .
O2 O 0.36915(9) 0.70381(9) 0.14673(10) 0.0319(3) Uani 1 1 d . . .
O3 O 0.27072(8) 0.59944(9) 0.30845(9) 0.0246(3) Uani 1 1 d . . .
O4 O 0.24987(8) 0.41697(9) 0.34729(9) 0.0237(3) Uani 1 1 d . . .
O1W O 0.39026(8) 0.81210(9) 0.35895(10) 0.0284(3) Uani 1 1 d . . .
H1WA H 0.4333 0.7633 0.3873 0.034 Uiso 1 1 d R . .
H1WB H 0.3884 0.8607 0.4073 0.034 Uiso 1 1 d R . .
O2W O 0.14310(10) 0.68563(10) 0.08569(11) 0.0443(4) Uani 1 1 d . . .
H2WA H 0.1417 0.6214 0.0586 0.053 Uiso 1 1 d R . .
H2WB H 0.1175 0.7316 0.0322 0.053 Uiso 1 1 d R . .
O3W O 0.37198(10) 0.96899(12) 0.53032(11) 0.0397(3) Uani 1 1 d . . .
H3WA H 0.3195 0.9828 0.5456 0.048 Uiso 1 1 d R . .
H3WB H 0.4203 0.9774 0.5909 0.048 Uiso 1 1 d R . .
O4W O 0.5000 0.95927(17) 0.2500 0.0426(5) Uani 1 2 d S . .
H4WA H 0.5484 0.9319 0.2347 0.051 Uiso 1 1 d 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
Mg1 0.0269(3) 0.0121(3) 0.0276(3) -0.00006(18) 0.0163(2) 0.00178(18)
C1 0.0191(7) 0.0169(7) 0.0214(7) -0.0031(6) 0.0105(6) -0.0007(5)
C2 0.0191(7) 0.0138(7) 0.0215(7) -0.0018(5) 0.0094(6) -0.0012(5)
C3 0.0412(9) 0.0155(7) 0.0414(9) -0.0071(6) 0.0276(8) -0.0011(7)
C4 0.0211(7) 0.0187(7) 0.0206(7) -0.0017(5) 0.0110(6) -0.0028(6)
C5 0.0186(7) 0.0145(7) 0.0189(7) -0.0003(5) 0.0080(5) 0.0001(5)
N1 0.0323(7) 0.0199(7) 0.0343(7) -0.0061(5) 0.0243(6) -0.0029(5)
N2 0.0301(7) 0.0142(6) 0.0317(7) -0.0036(5) 0.0188(6) -0.0023(5)
O1 0.0377(6) 0.0236(6) 0.0433(7) -0.0075(5) 0.0316(6) -0.0090(5)
O2 0.0442(7) 0.0170(6) 0.0480(7) 0.0032(5) 0.0341(6) 0.0033(5)
O3 0.0372(6) 0.0136(5) 0.0298(6) 0.0000(4) 0.0205(5) 0.0023(4)
O4 0.0343(6) 0.0159(5) 0.0282(6) 0.0006(4) 0.0204(5) -0.0023(4)
O1W 0.0308(6) 0.0216(6) 0.0325(6) -0.0035(5) 0.0097(5) 0.0054(5)
O2W 0.0559(8) 0.0241(6) 0.0408(7) 0.0051(5) -0.0023(6) -0.0044(6)
O3W 0.0383(7) 0.0500(8) 0.0339(7) -0.0063(6) 0.0159(5) 0.0053(6)
O4W 0.0335(9) 0.0444(11) 0.0534(11) 0.000 0.0185(9) 0.000

_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 O2 2.0139(12) . ?
Mg1 O3 2.0189(12) . ?
Mg1 O2W 2.0712(15) . ?
Mg1 O4 2.1137(12) 4 ?
Mg1 O1W 2.1491(14) . ?
Mg1 N2 2.1501(13) 4 ?
C1 N1 1.3688(19) . ?
C1 C2 1.382(2) . ?
C1 C4 1.491(2) . ?
C2 N2 1.3779(19) . ?
C2 C5 1.5006(19) . ?
C3 N2 1.316(2) . ?
C3 N1 1.336(2) . ?
C3 H3 0.9300 . ?
C4 O2 1.2442(18) . ?
C4 O1 1.2532(18) . ?
C5 O3 1.2504(18) . ?
C5 O4 1.2610(17) . ?
N1 H1A 0.8985 . ?
N2 Mg1 2.1501(13) 4_545 ?
O4 Mg1 2.1137(12) 4_545 ?
O1W H1WA 0.8191 . ?
O1W H1WB 0.8195 . ?
O2W H2WA 0.8143 . ?
O2W H2WB 0.8295 . ?
O3W H3WA 0.8241 . ?
O3W H3WB 0.8312 . ?
O4W H4WA 0.8177 . ?

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
O2 Mg1 O3 95.16(5) . . ?
O2 Mg1 O2W 94.88(6) . . ?
O3 Mg1 O2W 90.37(5) . . ?
O2 Mg1 O4 93.14(5) . 4 ?
O3 Mg1 O4 170.23(5) . 4 ?
O2W Mg1 O4 94.05(5) . 4 ?
O2 Mg1 O1W 84.11(5) . . ?
O3 Mg1 O1W 89.64(5) . . ?
O2W Mg1 O1W 178.98(6) . . ?
O4 Mg1 O1W 86.10(5) 4 . ?
O2 Mg1 N2 166.95(5) . 4 ?
O3 Mg1 N2 95.15(5) . 4 ?
O2W Mg1 N2 93.04(6) . 4 ?
O4 Mg1 N2 75.94(5) 4 4 ?
O1W Mg1 N2 87.98(5) . 4 ?
N1 C1 C2 104.97(12) . . ?
N1 C1 C4 118.78(12) . . ?
C2 C1 C4 136.24(13) . . ?
N2 C2 C1 109.27(12) . . ?
N2 C2 C5 115.32(12) . . ?
C1 C2 C5 135.31(13) . . ?
N2 C3 N1 111.30(13) . . ?
N2 C3 H3 124.4 . . ?
N1 C3 H3 124.4 . . ?
O2 C4 O1 123.55(14) . . ?
O2 C4 C1 120.06(12) . . ?
O1 C4 C1 116.38(13) . . ?
O3 C5 O4 123.68(13) . . ?
O3 C5 C2 121.45(13) . . ?
O4 C5 C2 114.87(12) . . ?
C3 N1 C1 108.51(12) . . ?
C3 N1 H1A 123.1 . . ?
C1 N1 H1A 128.4 . . ?
C3 N2 C2 105.94(12) . . ?
C3 N2 Mg1 141.02(11) . 4_545 ?
C2 N2 Mg1 112.41(9) . 4_545 ?
C4 O2 Mg1 143.50(10) . . ?
C5 O3 Mg1 139.03(10) . . ?
C5 O4 Mg1 117.90(9) . 4_545 ?
Mg1 O1W H1WA 113.7 . . ?
Mg1 O1W H1WB 126.3 . . ?
H1WA O1W H1WB 111.3 . . ?
Mg1 O2W H2WA 123.5 . . ?
Mg1 O2W H2WB 115.5 . . ?
H2WA O2W H2WB 109.2 . . ?
H3WA O3W H3WB 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -0.73(16) . . . . ?
C4 C1 C2 N2 179.10(16) . . . . ?
N1 C1 C2 C5 175.47(15) . . . . ?
C4 C1 C2 C5 -4.7(3) . . . . ?
N1 C1 C4 O2 168.32(14) . . . . ?
C2 C1 C4 O2 -11.5(3) . . . . ?
N1 C1 C4 O1 -10.7(2) . . . . ?
C2 C1 C4 O1 169.53(16) . . . . ?
N2 C2 C5 O3 -176.44(13) . . . . ?
C1 C2 C5 O3 7.5(2) . . . . ?
N2 C2 C5 O4 3.72(18) . . . . ?
C1 C2 C5 O4 -172.32(15) . . . . ?
N2 C3 N1 C1 -0.48(19) . . . . ?
C2 C1 N1 C3 0.73(17) . . . . ?
C4 C1 N1 C3 -179.14(14) . . . . ?
N1 C3 N2 C2 0.01(19) . . . . ?
N1 C3 N2 Mg1 169.47(13) . . . 4_545 ?
C1 C2 N2 C3 0.46(17) . . . . ?
C5 C2 N2 C3 -176.59(13) . . . . ?
C1 C2 N2 Mg1 -172.39(9) . . . 4_545 ?
C5 C2 N2 Mg1 10.57(15) . . . 4_545 ?
O1 C4 O2 Mg1 176.42(13) . . . . ?
C1 C4 O2 Mg1 -2.5(3) . . . . ?
O3 Mg1 O2 C4 23.20(19) . . . . ?
O2W Mg1 O2 C4 -67.61(19) . . . . ?
O4 Mg1 O2 C4 -161.95(18) 4 . . . ?
O1W Mg1 O2 C4 112.30(19) . . . . ?
N2 Mg1 O2 C4 165.3(2) 4 . . . ?
O4 C5 O3 Mg1 -155.19(11) . . . . ?
C2 C5 O3 Mg1 25.0(2) . . . . ?
O2 Mg1 O3 C5 -38.21(16) . . . . ?
O2W Mg1 O3 C5 56.72(16) . . . . ?
O4 Mg1 O3 C5 173.7(3) 4 . . . ?
O1W Mg1 O3 C5 -122.26(16) . . . . ?
N2 Mg1 O3 C5 149.81(16) 4 . . . ?
O3 C5 O4 Mg1 163.14(11) . . . 4_545 ?
C2 C5 O4 Mg1 -17.02(15) . . . 4_545 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.19
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.051


