# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_journal_volume ?
_journal_page_first ?
_journal_year ?
_publ_contact_author_name 'Christoph Janiak'
_publ_contact_author_email JANIAK@UNI-FREIBURG.DE
_publ_section_title
;
2\/Y[Cu2(\m5-btb)(\m-OH)(\m-H2O)] a two-dimensional
coordination polymer built from ferromagnetically coupled Cu2
units (btb = benzene-1,2,3-tricarboxylate)
;
loop_
_publ_author_name
'Christoph Janiak'
'Hesham A Habib'
'Joaquin Sanchiz'
# Attachment '1-new.cif'
data_m500
_database_code_depnum_ccdc_archive 'CCDC 680410'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-[aqua(\mu5-benzene-1,2,3-tricarboxylato-
\kO:\kO':\kO'':\kO''':\kO'''',O''''')(\mu-hydroxo)dicopper(II)]
;
_chemical_name_common
;
catena-(aqua(muu5-benzene-1,2,3-tricarboxylato-
kappaO:kappaO':kappaO'':kappaO''':kappaO'''',O''''')(muu-
hydroxo)dicopper(ii))
;
_chemical_melting_point ?
_chemical_formula_moiety 'C9 H6 Cu2 O8'
_chemical_formula_sum 'C9 H6 Cu2 O8'
_chemical_formula_weight 369.22
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 5.68200(10)
_cell_length_b 27.2143(6)
_cell_length_c 6.7260(2)
_cell_angle_alpha 90.00
_cell_angle_beta 107.6180(10)
_cell_angle_gamma 90.00
_cell_volume 991.27(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 2177
_cell_measurement_theta_min 2.86
_cell_measurement_theta_max 27.19
_exptl_crystal_description plate
_exptl_crystal_colour green
_exptl_crystal_size_max 0.13
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.474
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 728
_exptl_absorpt_coefficient_mu 4.329
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5947
_exptl_absorpt_correction_T_max 0.9499
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 203(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 area detector'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 7609
_diffrn_reflns_av_R_equivalents 0.0452
_diffrn_reflns_av_sigmaI/netI 0.0384
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_k_max 33
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_theta_min 1.50
_diffrn_reflns_theta_max 26.35
_reflns_number_total 2015
_reflns_number_gt 1706
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH) and refined using a
riding model (AFIX 43 for aromatic CH),
with U~iso~(H) = 1.2U~eq~(CH)
Hydrogen atoms on the aqua and hydroxo ligand were found and refined with
U~iso~(H) = 1.5U~eq~(O).
The hydrogen atoms H7 on the hydroxo ligand O7 and H8A on the aqua ligand
were constrained with DFIX to
O---H = 0.90(5) \%A.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0323P)^2^+0.5993P] where P=(Fo^2^+2Fc^2^)/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 2015
_refine_ls_number_parameters 181
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0391
_refine_ls_R_factor_gt 0.0286
_refine_ls_wR_factor_ref 0.0682
_refine_ls_wR_factor_gt 0.0647
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_restrained_S_all 1.064
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.22501(7) 0.231094(15) 0.46642(6) 0.00938(12) Uani 1 1 d . . .
Cu2 Cu 0.45234(7) 0.138290(15) 0.33569(6) 0.01042(12) Uani 1 1 d . . .
O7 O 0.5295(4) 0.20047(9) 0.4750(4) 0.0095(5) Uani 1 1 d D . .
H7 H 0.601(7) 0.1981(16) 0.589(5) 0.014 Uiso 1 1 d D . .
O8 O -0.1237(4) 0.24983(10) 0.3719(4) 0.0131(5) Uani 1 1 d D . .
H8A H -0.152(8) 0.2768(14) 0.405(7) 0.020 Uiso 1 1 d D . .
H8B H -0.201(8) 0.2307(17) 0.406(7) 0.020 Uiso 1 1 d . . .
C1 C -0.0067(6) 0.10062(13) 0.7053(5) 0.0124(7) Uani 1 1 d . . .
C2 C -0.0967(6) 0.11943(12) 0.8635(5) 0.0091(6) Uani 1 1 d . . .
C3 C -0.2413(6) 0.08806(13) 0.9441(5) 0.0121(7) Uani 1 1 d . . .
C4 C -0.2923(7) 0.04012(14) 0.8724(7) 0.0234(9) Uani 1 1 d . . .
H4 H -0.3902 0.0200 0.9289 0.028 Uiso 1 1 calc R . .
C5 C -0.2006(8) 0.02179(15) 0.7188(7) 0.0312(10) Uani 1 1 d . . .
H5 H -0.2331 -0.0108 0.6716 0.037 Uiso 1 1 calc R . .
C6 C -0.0596(7) 0.05261(14) 0.6358(6) 0.0206(8) Uani 1 1 d . . .
H6 H 0.0017 0.0407 0.5300 0.025 Uiso 1 1 calc R . .
C7 C 0.1338(6) 0.13131(12) 0.5950(5) 0.0087(6) Uani 1 1 d . . .
O1 O 0.1230(4) 0.17704(9) 0.6146(4) 0.0121(5) Uani 1 1 d . . .
O2 O 0.2488(4) 0.10890(9) 0.4871(4) 0.0151(5) Uani 1 1 d . . .
C8 C -0.0415(6) 0.17169(12) 0.9487(5) 0.0078(6) Uani 1 1 d . . .
O3 O -0.2102(4) 0.20317(8) 0.8726(3) 0.0099(5) Uani 1 1 d . . .
O4 O 0.1577(4) 0.18036(9) 1.0857(4) 0.0131(5) Uani 1 1 d . . .
C9 C -0.3517(6) 0.10528(12) 1.1071(5) 0.0107(7) Uani 1 1 d . . .
O5 O -0.5103(4) 0.07966(9) 1.1577(4) 0.0180(5) Uani 1 1 d . . .
O6 O -0.2905(4) 0.14632(9) 1.1951(4) 0.0163(5) Uani 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
Cu1 0.0077(2) 0.0086(2) 0.0138(2) 0.00313(16) 0.00614(15) 0.00083(15)
Cu2 0.0125(2) 0.0107(2) 0.0118(2) -0.00163(16) 0.00913(16) -0.00134(15)
O7 0.0090(11) 0.0132(12) 0.0061(11) 0.0007(9) 0.0020(9) 0.0012(9)
O8 0.0109(12) 0.0094(12) 0.0221(14) 0.0032(11) 0.0099(10) -0.0007(10)
C1 0.0150(16) 0.0133(17) 0.0126(17) -0.0006(13) 0.0095(13) 0.0025(13)
C2 0.0083(15) 0.0099(16) 0.0098(16) -0.0002(12) 0.0038(12) 0.0005(12)
C3 0.0131(16) 0.0116(16) 0.0140(17) -0.0024(13) 0.0079(13) 0.0005(13)
C4 0.037(2) 0.0126(18) 0.033(2) -0.0047(16) 0.0290(19) -0.0078(16)
C5 0.048(3) 0.014(2) 0.048(3) -0.0122(19) 0.038(2) -0.0133(18)
C6 0.036(2) 0.0129(18) 0.025(2) -0.0043(15) 0.0265(17) -0.0023(15)
C7 0.0079(15) 0.0095(16) 0.0093(16) 0.0000(12) 0.0036(12) -0.0010(12)
O1 0.0144(12) 0.0109(12) 0.0144(12) 0.0007(9) 0.0093(10) -0.0006(9)
O2 0.0217(13) 0.0121(12) 0.0185(13) -0.0008(10) 0.0168(11) -0.0012(10)
C8 0.0102(15) 0.0096(15) 0.0069(15) 0.0020(12) 0.0076(12) -0.0005(12)
O3 0.0110(11) 0.0093(11) 0.0099(11) -0.0038(9) 0.0038(9) 0.0007(9)
O4 0.0107(12) 0.0128(12) 0.0145(13) -0.0003(9) 0.0019(10) -0.0020(9)
C9 0.0113(16) 0.0107(16) 0.0132(17) 0.0026(13) 0.0081(13) 0.0029(12)
O5 0.0228(13) 0.0157(13) 0.0236(14) -0.0060(10) 0.0194(11) -0.0058(10)
O6 0.0196(13) 0.0165(13) 0.0179(13) -0.0070(10) 0.0134(11) -0.0050(10)
_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
Cu1 O7 1.905(2) . ?
Cu1 O8 1.956(2) . ?
Cu1 O1 1.960(2) . ?
Cu1 O3 1.968(2) 4_665 ?
Cu2 O7 1.920(2) . ?
Cu2 O2 1.931(2) . ?
Cu2 O6 1.978(2) 1_654 ?
Cu2 O5 2.044(2) 1_654 ?
Cu2 O4 2.288(2) 1_554 ?
Cu2 C9 2.334(3) 1_654 ?
O7 H7 0.76(3) . ?
O8 H8A 0.80(4) . ?
O8 H8B 0.76(5) . ?
C1 C6 1.390(5) . ?
C1 C2 1.409(5) . ?
C1 C7 1.497(5) . ?
C2 C3 1.403(5) . ?
C2 C8 1.530(4) . ?
C3 C4 1.391(5) . ?
C3 C9 1.494(5) . ?
C4 C5 1.383(5) . ?
C4 H4 0.9400 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9400 . ?
C6 H6 0.9400 . ?
C7 O1 1.255(4) . ?
C7 O2 1.270(4) . ?
C8 O4 1.247(4) . ?
C8 O3 1.272(4) . ?
O3 Cu1 1.968(2) 4_566 ?
O4 Cu2 2.289(2) 1_556 ?
C9 O6 1.262(4) . ?
C9 O5 1.265(4) . ?
C9 Cu2 2.334(3) 1_456 ?
O5 Cu2 2.044(2) 1_456 ?
O6 Cu2 1.978(2) 1_456 ?
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
O7 Cu1 O8 160.89(11) . . ?
O7 Cu1 O1 93.55(10) . . ?
O8 Cu1 O1 86.24(10) . . ?
O7 Cu1 O3 98.69(10) . 4_665 ?
O8 Cu1 O3 85.89(10) . 4_665 ?
O1 Cu1 O3 163.27(10) . 4_665 ?
O7 Cu2 O2 101.10(10) . . ?
O7 Cu2 O6 92.49(10) . 1_654 ?
O2 Cu2 O6 160.90(11) . 1_654 ?
O7 Cu2 O5 157.69(10) . 1_654 ?
O2 Cu2 O5 99.82(10) . 1_654 ?
O6 Cu2 O5 65.39(10) 1_654 1_654 ?
O7 Cu2 O4 85.75(9) . 1_554 ?
O2 Cu2 O4 99.97(9) . 1_554 ?
O6 Cu2 O4 94.33(10) 1_654 1_554 ?
O5 Cu2 O4 98.20(9) 1_654 1_554 ?
O7 Cu2 C9 125.23(11) . 1_654 ?
O2 Cu2 C9 132.03(11) . 1_654 ?
O6 Cu2 C9 32.74(11) 1_654 1_654 ?
O5 Cu2 C9 32.74(11) 1_654 1_654 ?
O4 Cu2 C9 95.58(10) 1_554 1_654 ?
Cu1 O7 Cu2 107.43(11) . . ?
Cu1 O7 H7 106(3) . . ?
Cu2 O7 H7 113(3) . . ?
Cu1 O8 H8A 115(3) . . ?
Cu1 O8 H8B 110(3) . . ?
H8A O8 H8B 111(5) . . ?
C6 C1 C2 120.3(3) . . ?
C6 C1 C7 116.9(3) . . ?
C2 C1 C7 122.8(3) . . ?
C3 C2 C1 117.4(3) . . ?
C3 C2 C8 119.9(3) . . ?
C1 C2 C8 122.7(3) . . ?
C4 C3 C2 121.5(3) . . ?
C4 C3 C9 117.3(3) . . ?
C2 C3 C9 121.2(3) . . ?
C5 C4 C3 120.8(3) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.4(4) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C5 C6 C1 121.7(3) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
O1 C7 O2 125.9(3) . . ?
O1 C7 C1 116.8(3) . . ?
O2 C7 C1 117.3(3) . . ?
C7 O1 Cu1 131.3(2) . . ?
C7 O2 Cu2 126.6(2) . . ?
O4 C8 O3 125.1(3) . . ?
O4 C8 C2 119.4(3) . . ?
O3 C8 C2 115.5(3) . . ?
C8 O3 Cu1 132.4(2) . 4_566 ?
C8 O4 Cu2 138.3(2) . 1_556 ?
O6 C9 O5 118.6(3) . . ?
O6 C9 C3 120.3(3) . . ?
O5 C9 C3 121.1(3) . . ?
O6 C9 Cu2 57.95(17) . 1_456 ?
O5 C9 Cu2 60.93(17) . 1_456 ?
C3 C9 Cu2 173.9(2) . 1_456 ?
C9 O5 Cu2 86.3(2) . 1_456 ?
C9 O6 Cu2 89.3(2) . 1_456 ?
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
O7 H7 O3 0.76(3) 1.89(3) 2.636(3) 171(5) 1_655
O8 H8A O4 0.80(4) 2.19(4) 2.881(3) 145(4) 4_565
O8 H8B O7 0.76(5) 1.91(5) 2.645(3) 161(5) 1_455
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 26.35
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.546
_refine_diff_density_min -0.518
_refine_diff_density_rms 0.114
# Attachment '2_fin.CIF'
data_m66
_database_code_depnum_ccdc_archive 'CCDC 680411'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
[tetraaqua-bis(dihydrogen-benzene-1,2,3-
tricarboxylato-\kO'')cadmium(II)] dihydrate
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C18 H18 Cd O16, 2(H2 O)'
_chemical_formula_sum 'C18 H22 Cd O18'
_chemical_formula_weight 638.76
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'
Cd Cd -0.8075 1.2024 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_Symmetry_space_group_name_Hall '-C 2yc'
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 29.6359(6)
_cell_length_b 6.58730(10)
_cell_length_c 11.7026(2)
_cell_angle_alpha 90.00
_cell_angle_beta 95.654(2)
_cell_angle_gamma 90.00
_cell_volume 2273.47(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 9978
_cell_measurement_theta_min 2.76
_cell_measurement_theta_max 33.87
_exptl_crystal_description plate
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.866
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1288
_exptl_absorpt_coefficient_mu 1.053
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.7030
_exptl_absorpt_correction_T_max 0.8666
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 203(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 area detector'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 24112
_diffrn_reflns_av_R_equivalents 0.0288
_diffrn_reflns_av_sigmaI/netI 0.0177
_diffrn_reflns_limit_h_min -41
_diffrn_reflns_limit_h_max 41
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.76
_diffrn_reflns_theta_max 29.85
_reflns_number_total 3265
_reflns_number_gt 3001
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH) and refined using a
riding model (AFIX 43 for aromatic CH),
with U~iso~(H) = 1.2U~eq~(CH)
Hydrogen atoms on the aqua ligands, the crystal water and the protonated
carboxylate groups were found and refined with
U~iso~(H) = 1.5U~eq~(O).
The bond O2---H2B had to be constrained with DFIX 0.8(2) in order
not to become shorter than 0.70 \%A.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0338P)^2^+2.6779P] where P=(Fo^2^+2Fc^2^)/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 3265
_refine_ls_number_parameters 192
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0282
_refine_ls_R_factor_gt 0.0246
_refine_ls_wR_factor_ref 0.0636
_refine_ls_wR_factor_gt 0.0620
_refine_ls_goodness_of_fit_ref 1.101
_refine_ls_restrained_S_all 1.101
_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
Cd Cd 0.0000 0.05337(3) 0.2500 0.01879(6) Uani 1 2 d S . .
O1 O 0.01212(5) 0.2933(2) 0.40065(12) 0.0271(3) Uani 1 1 d . . .
H1A H -0.0063(10) 0.362(5) 0.378(3) 0.041 Uiso 1 1 d . . .
H1B H 0.0374(10) 0.343(5) 0.406(2) 0.041 Uiso 1 1 d . . .
O2 O -0.01824(5) -0.1953(3) 0.11717(12) 0.0299(3) Uani 1 1 d D . .
H2A H -0.0446(10) -0.197(5) 0.093(2) 0.045 Uiso 1 1 d . . .
H2B H -0.0029(9) -0.207(5) 0.068(2) 0.045 Uiso 1 1 d D . .
O11 O 0.16904(4) 0.2672(2) -0.07385(11) 0.0243(3) Uani 1 1 d . . .
H11 H 0.1530(9) 0.263(4) -0.137(2) 0.036 Uiso 1 1 d . . .
O12 O 0.10401(4) 0.1768(3) -0.00711(11) 0.0295(3) Uani 1 1 d . . .
O13 O 0.07356(4) 0.07994(19) 0.22531(11) 0.0186(2) Uani 1 1 d . . .
O14 O 0.07216(4) 0.41323(19) 0.19124(12) 0.0216(3) Uani 1 1 d . . .
O15 O 0.10491(4) 0.3299(3) 0.43710(11) 0.0281(3) Uani 1 1 d . . .
O16 O 0.16997(4) 0.2351(2) 0.53347(11) 0.0252(3) Uani 1 1 d . . .
H16 H 0.1530(9) 0.243(4) 0.584(2) 0.038 Uiso 1 1 d . . .
C11 C 0.16784(5) 0.2406(3) 0.12646(13) 0.0166(3) Uani 1 1 d . . .
C12 C 0.14363(5) 0.2492(2) 0.22346(13) 0.0143(3) Uani 1 1 d . . .
C13 C 0.16798(5) 0.2570(3) 0.33212(13) 0.0171(3) Uani 1 1 d . . .
C14 C 0.21528(6) 0.2544(3) 0.34244(15) 0.0259(4) Uani 1 1 d . . .
H14 H 0.2314 0.2585 0.4158 0.031 Uiso 1 1 calc R . .
C15 C 0.23877(6) 0.2458(4) 0.24646(16) 0.0315(5) Uani 1 1 d . . .
H15 H 0.2706 0.2441 0.2543 0.038 Uiso 1 1 calc R . .
C16 C 0.21509(6) 0.2398(3) 0.13896(15) 0.0253(4) Uani 1 1 d . . .
H16A H 0.2310 0.2352 0.0734 0.030 Uiso 1 1 calc R . .
C17 C 0.14332(6) 0.2260(3) 0.00906(14) 0.0184(3) Uani 1 1 d . . .
C18 C 0.09206(5) 0.2506(3) 0.21152(13) 0.0159(3) Uani 1 1 d . . .
C19 C 0.14391(6) 0.2764(3) 0.43804(14) 0.0186(3) Uani 1 1 d . . .
O3 O 0.12468(4) 0.7440(2) 0.21857(10) 0.0190(2) Uani 1 1 d . . .
H5A H 0.1083(9) 0.650(5) 0.209(2) 0.029 Uiso 1 1 d . . .
H5B H 0.1103(9) 0.838(5) 0.213(2) 0.029 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
Cd 0.01301(8) 0.02707(11) 0.01632(8) 0.000 0.00155(5) 0.000
O1 0.0199(6) 0.0339(8) 0.0274(7) -0.0019(6) 0.0029(5) 0.0022(6)
O2 0.0235(6) 0.0406(9) 0.0253(6) -0.0091(6) 0.0000(5) -0.0005(6)
O11 0.0224(6) 0.0370(8) 0.0136(5) 0.0015(5) 0.0024(5) -0.0018(5)
O12 0.0218(6) 0.0474(9) 0.0187(6) -0.0004(6) -0.0010(5) -0.0084(6)
O13 0.0153(5) 0.0184(6) 0.0224(6) 0.0001(5) 0.0034(4) -0.0014(4)
O14 0.0182(5) 0.0181(6) 0.0280(6) 0.0014(5) 0.0000(5) 0.0019(4)
O15 0.0201(6) 0.0443(9) 0.0202(6) -0.0035(6) 0.0027(5) 0.0038(6)
O16 0.0227(6) 0.0389(8) 0.0139(5) 0.0026(5) 0.0017(5) 0.0025(6)
C11 0.0167(7) 0.0187(8) 0.0144(6) 0.0007(6) 0.0021(5) -0.0007(6)
C12 0.0138(6) 0.0135(7) 0.0155(6) 0.0005(5) 0.0011(5) -0.0011(5)
C13 0.0163(7) 0.0205(8) 0.0146(6) 0.0000(6) 0.0017(5) -0.0005(6)
C14 0.0168(7) 0.0420(11) 0.0180(7) 0.0000(7) -0.0027(6) -0.0016(7)
C15 0.0140(7) 0.0570(14) 0.0232(8) 0.0009(9) 0.0008(6) -0.0010(8)
C16 0.0170(7) 0.0416(11) 0.0180(7) 0.0006(7) 0.0048(6) -0.0012(7)
C17 0.0200(7) 0.0197(8) 0.0154(7) -0.0005(6) 0.0016(6) 0.0007(6)
C18 0.0146(7) 0.0193(8) 0.0137(6) -0.0005(6) 0.0012(5) -0.0003(6)
C19 0.0197(7) 0.0207(8) 0.0154(7) -0.0015(6) 0.0015(6) -0.0027(6)
O3 0.0206(6) 0.0178(6) 0.0184(5) -0.0005(5) 0.0009(4) -0.0004(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
Cd O13 2.2339(12) . ?
Cd O13 2.2339(12) 2 ?
Cd O2 2.2862(15) . ?
Cd O2 2.2862(15) 2 ?
Cd O1 2.3687(15) . ?
Cd O1 2.3687(15) 2 ?
O1 H1A 0.74(3) . ?
O1 H1B 0.82(3) . ?
O2 H2A 0.81(3) . ?
O2 H2B 0.770(17) . ?
O11 C17 1.320(2) . ?
O11 H11 0.84(3) . ?
O12 C17 1.206(2) . ?
O13 C18 1.268(2) . ?
O14 C18 1.235(2) . ?
O15 C19 1.207(2) . ?
O16 C19 1.322(2) . ?
O16 H16 0.82(3) . ?
C11 C16 1.394(2) . ?
C11 C12 1.402(2) . ?
C11 C17 1.493(2) . ?
C12 C13 1.400(2) . ?
C12 C18 1.521(2) . ?
C13 C14 1.395(2) . ?
C13 C19 1.495(2) . ?
C14 C15 1.380(3) . ?
C14 H14 0.9400 . ?
C15 C16 1.379(2) . ?
C15 H15 0.9400 . ?
C16 H16A 0.9400 . ?
O3 H5A 0.79(3) . ?
O3 H5B 0.75(3) . ?
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
O13 Cd O13 171.01(6) . 2 ?
O13 Cd O2 97.85(5) . . ?
O13 Cd O2 88.61(5) 2 . ?
O13 Cd O2 88.61(5) . 2 ?
O13 Cd O2 97.85(5) 2 2 ?
O2 Cd O2 88.46(8) . 2 ?
O13 Cd O1 88.03(5) . . ?
O13 Cd O1 85.97(5) 2 . ?
O2 Cd O1 173.02(5) . . ?
O2 Cd O1 87.92(6) 2 . ?
O13 Cd O1 85.97(5) . 2 ?
O13 Cd O1 88.03(5) 2 2 ?
O2 Cd O1 87.92(6) . 2 ?
O2 Cd O1 173.02(5) 2 2 ?
O1 Cd O1 96.29(8) . 2 ?
Cd O1 H1A 95(2) . . ?
Cd O1 H1B 113(2) . . ?
H1A O1 H1B 115(3) . . ?
Cd O2 H2A 114(2) . . ?
Cd O2 H2B 117(2) . . ?
H2A O2 H2B 111(3) . . ?
C17 O11 H11 108.8(19) . . ?
C18 O13 Cd 121.72(10) . . ?
C19 O16 H16 104.7(19) . . ?
C16 C11 C12 120.27(15) . . ?
C16 C11 C17 119.30(15) . . ?
C12 C11 C17 120.41(14) . . ?
C13 C12 C11 118.53(14) . . ?
C13 C12 C18 120.44(14) . . ?
C11 C12 C18 121.03(14) . . ?
C14 C13 C12 120.12(15) . . ?
C14 C13 C19 119.12(15) . . ?
C12 C13 C19 120.71(14) . . ?
C15 C14 C13 120.88(16) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C16 C15 C14 119.44(16) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C11 120.75(16) . . ?
C15 C16 H16A 119.6 . . ?
C11 C16 H16A 119.6 . . ?
O12 C17 O11 123.98(15) . . ?
O12 C17 C11 122.47(15) . . ?
O11 C17 C11 113.54(14) . . ?
O14 C18 O13 126.12(15) . . ?
O14 C18 C12 118.65(15) . . ?
O13 C18 C12 115.23(14) . . ?
O15 C19 O16 123.16(15) . . ?
O15 C19 C13 123.50(15) . . ?
O16 C19 C13 113.31(14) . . ?
H5A O3 H5B 108(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
O1 H1A O14 0.74(3) 2.07(3) 2.737(2) 152(3) 2
O1 H1B O15 0.82(3) 2.00(3) 2.752(2) 153(3) .
O2 H2A O12 0.81(3) 1.94(3) 2.7366(19) 169(3) 5
O2 H2B O1 0.770(17) 2.13(2) 2.845(2) 155(3) 6
O11 H11 O3 0.84(3) 1.81(3) 2.6469(18) 173(3) 6_565
O16 H16 O3 0.82(3) 1.85(3) 2.6619(18) 169(3) 6_566
O3 H5A O14 0.79(3) 1.89(3) 2.6785(19) 176(3) .
O3 H5B O13 0.75(3) 1.94(3) 2.6874(19) 171(3) 1_565
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 29.85
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.223
_refine_diff_density_min -0.389
_refine_diff_density_rms 0.086