data_STAM1
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C30 H18 Cu3 O18,8(H2 O)'
_chemical_formula_sum
'C30 H34 Cu3 O26'
_chemical_formula_weight 1001.19
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 Trigonal
_symmetry_space_group_name_H-M P-3m1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
_cell_length_a 18.6781(19)
_cell_length_b 18.6781(19)
_cell_length_c 6.8358(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 2065.3(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 93(2)
_cell_measurement_reflns_used 8255
_cell_measurement_theta_min 6.47
_cell_measurement_theta_max 54.77
_exptl_crystal_description Prism
_exptl_crystal_colour Blue
_exptl_crystal_size_max 0.06
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.610
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1018
_exptl_absorpt_coefficient_mu 1.622
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.9089
_exptl_absorpt_correction_T_max 0.9380
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 93(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_monochromator confocal
_diffrn_measurement_device_type CCD
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 0.83
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 14411
_diffrn_reflns_av_R_equivalents 0.0363
_diffrn_reflns_av_sigmaI/netI 0.0229
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_theta_min 3.24
_diffrn_reflns_theta_max 27.39
_reflns_number_total 1631
_reflns_number_gt 1457
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku Corp., 2004)'
_computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Ortep-3'
_computing_publication_material 'Bruker SHELXTL'
_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^)+(0.0558P)^2^+3.7008P] 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 constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1631
_refine_ls_number_parameters 106
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0450
_refine_ls_R_factor_gt 0.0395
_refine_ls_wR_factor_ref 0.1127
_refine_ls_wR_factor_gt 0.1089
_refine_ls_goodness_of_fit_ref 1.129
_refine_ls_restrained_S_all 1.129
_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
C7 C 0.7651(8) 0.9553(8) 0.0751(15) 0.086(4) Uani 0.50 1 d P . .
Cu1 Cu 0.523168(13) 0.476832(13) 0.84273(6) 0.01533(18) Uani 1 2 d S . .
O3 O 0.55786(14) 0.58911(12) 0.7499(3) 0.0265(5) Uani 1 1 d . . .
C1 C 0.54993(18) 0.64129(19) 0.8510(4) 0.0212(6) Uani 1 1 d . . .
C2 C 0.57792(17) 0.72439(18) 0.7621(4) 0.0204(6) Uani 1 1 d . . .
O2 O 0.4807(2) 0.37131(16) 0.9805(3) 0.0508(8) Uani 1 1 d . . .
C4 C 0.62467(19) 0.74777(19) 0.5897(4) 0.0261(6) Uani 1 1 d . . .
H4 H 0.6396 0.7113 0.5295 0.031 Uiso 1 1 calc R . .
C5 C 0.6491(3) 0.82453(15) 0.5071(6) 0.0286(9) Uani 1 2 d S . .
C3 C 0.5559(2) 0.77793(12) 0.8484(5) 0.0189(8) Uani 1 2 d S . .
H3 H 0.5254 0.7627 0.9673 0.023 Uiso 1 2 calc SR . .
O1 O 0.56267(10) 0.43733(10) 0.5890(4) 0.0476(11) Uani 1 2 d S . .
C6 C 0.7014(3) 0.85070(17) 0.3265(7) 0.0411(13) Uani 1 2 d S . .
O4 O 0.7204(3) 0.9205(2) 0.2544(5) 0.0789(12) Uani 1 1 d . . .
O6 O 0.6667 0.3333 0.3606(11) 0.064(2) Uani 1 6 d S . .
O7 O 0.72834(12) 0.4567(2) 0.6620(5) 0.0420(8) Uani 1 2 d S . .
O5 O 0.6667 0.3333 0.9498(10) 0.0549(19) Uani 1 6 d S . .
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
C7 0.089(8) 0.116(10) 0.050(5) 0.040(6) 0.037(5) 0.048(8)
Cu1 0.0220(2) 0.0220(2) 0.0114(3) 0.00032(7) -0.00032(7) 0.0181(2)
O3 0.0331(11) 0.0191(10) 0.0249(10) 0.0008(8) 0.0072(9) 0.0112(9)
C1 0.0243(14) 0.0304(15) 0.0186(13) 0.0027(11) -0.0007(10) 0.0210(12)
C2 0.0205(13) 0.0238(15) 0.0201(13) 0.0043(10) 0.0028(10) 0.0136(12)
O2 0.109(2) 0.0462(15) 0.0297(12) 0.0245(11) 0.0353(14) 0.0626(17)
C4 0.0312(16) 0.0316(16) 0.0241(14) 0.0048(12) 0.0079(12) 0.0222(14)
C5 0.032(2) 0.0315(17) 0.022(2) 0.0058(9) 0.0116(18) 0.0161(12)
C3 0.0192(19) 0.0222(14) 0.0142(16) 0.0007(7) 0.0013(14) 0.0096(9)
O1 0.089(2) 0.089(2) 0.0137(14) -0.0014(6) 0.0014(6) 0.081(3)
C6 0.050(3) 0.045(2) 0.030(3) 0.0110(11) 0.022(2) 0.0248(16)
O4 0.106(3) 0.062(2) 0.0564(18) 0.0332(16) 0.054(2) 0.032(2)
O6 0.077(3) 0.077(3) 0.038(4) 0.000 0.000 0.0385(17)
O7 0.0365(14) 0.047(2) 0.046(2) 0.0042(17) 0.0021(8) 0.0233(11)
O5 0.066(3) 0.066(3) 0.033(3) 0.000 0.000 0.0330(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
C7 O4 1.442(9) . ?
C7 C7 1.77(2) 5_675 ?
Cu1 O2 1.959(2) 10_665 ?
Cu1 O2 1.959(2) . ?
Cu1 O3 1.965(2) . ?
Cu1 O3 1.965(2) 10_665 ?
Cu1 O1 2.155(3) . ?
Cu1 Cu1 2.6211(9) 7_667 ?
O3 C1 1.263(3) . ?
C1 O2 1.255(4) 7_667 ?
C1 C2 1.497(4) . ?
C2 C3 1.389(3) . ?
C2 C4 1.401(4) . ?
O2 C1 1.255(4) 7_667 ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C4 1.389(4) 12_565 ?
C5 C6 1.497(6) . ?
C3 C2 1.389(3) 12_565 ?
C3 H3 0.9500 . ?
C6 O4 1.267(4) 12_565 ?
C6 O4 1.267(4) . ?
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
O4 C7 C7 144.2(12) . 5_675 ?
O2 Cu1 O2 89.7(2) 10_665 . ?
O2 Cu1 O3 89.72(12) 10_665 . ?
O2 Cu1 O3 168.69(9) . . ?
O2 Cu1 O3 168.69(9) 10_665 10_665 ?
O2 Cu1 O3 89.72(12) . 10_665 ?
O3 Cu1 O3 88.61(13) . 10_665 ?
O2 Cu1 O1 94.49(9) 10_665 . ?
O2 Cu1 O1 94.49(9) . . ?
O3 Cu1 O1 96.81(8) . . ?
O3 Cu1 O1 96.81(8) 10_665 . ?
O2 Cu1 Cu1 84.45(7) 10_665 7_667 ?
O2 Cu1 Cu1 84.45(7) . 7_667 ?
O3 Cu1 Cu1 84.25(6) . 7_667 ?
O3 Cu1 Cu1 84.25(6) 10_665 7_667 ?
O1 Cu1 Cu1 178.51(9) . 7_667 ?
C1 O3 Cu1 122.92(18) . . ?
O2 C1 O3 125.2(3) 7_667 . ?
O2 C1 C2 117.2(3) 7_667 . ?
O3 C1 C2 117.6(2) . . ?
C3 C2 C4 119.7(3) . . ?
C3 C2 C1 119.9(2) . . ?
C4 C2 C1 120.3(2) . . ?
C1 O2 Cu1 123.2(2) 7_667 . ?
C5 C4 C2 119.7(3) . . ?
C5 C4 H4 120.1 . . ?
C2 C4 H4 120.1 . . ?
C4 C5 C4 120.5(4) . 12_565 ?
C4 C5 C6 119.73(19) . . ?
C4 C5 C6 119.73(19) 12_565 . ?
C2 C3 C2 120.5(3) . 12_565 ?
C2 C3 H3 119.8 . . ?
C2 C3 H3 119.8 12_565 . ?
O4 C6 O4 125.4(5) 12_565 . ?
O4 C6 C5 117.3(2) 12_565 . ?
O4 C6 C5 117.3(2) . . ?
C6 O4 C7 126.6(6) . . ?
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
O2 Cu1 O3 C1 -83.8(2) 10_665 . . . ?
O2 Cu1 O3 C1 3.4(7) . . . . ?
O3 Cu1 O3 C1 85.0(2) 10_665 . . . ?
O1 Cu1 O3 C1 -178.3(2) . . . . ?
Cu1 Cu1 O3 C1 0.6(2) 7_667 . . . ?
Cu1 O3 C1 O2 -0.4(4) . . . 7_667 ?
Cu1 O3 C1 C2 -179.28(18) . . . . ?
O2 C1 C2 C3 -11.9(4) 7_667 . . . ?
O3 C1 C2 C3 167.1(3) . . . . ?
O2 C1 C2 C4 169.6(3) 7_667 . . . ?
O3 C1 C2 C4 -11.4(4) . . . . ?
O2 Cu1 O2 C1 83.8(3) 10_665 . . 7_667 ?
O3 Cu1 O2 C1 -3.4(8) . . . 7_667 ?
O3 Cu1 O2 C1 -84.9(3) 10_665 . . 7_667 ?
O1 Cu1 O2 C1 178.3(3) . . . 7_667 ?
Cu1 Cu1 O2 C1 -0.7(3) 7_667 . . 7_667 ?
C3 C2 C4 C5 0.5(5) . . . . ?
C1 C2 C4 C5 178.9(3) . . . . ?
C2 C4 C5 C4 -2.6(7) . . . 12_565 ?
C2 C4 C5 C6 178.0(4) . . . . ?
C4 C2 C3 C2 1.7(6) . . . 12_565 ?
C1 C2 C3 C2 -176.8(2) . . . 12_565 ?
C4 C5 C6 O4 1.0(8) . . . 12_565 ?
C4 C5 C6 O4 -178.4(5) 12_565 . . 12_565 ?
C4 C5 C6 O4 178.4(5) . . . . ?
C4 C5 C6 O4 -1.0(8) 12_565 . . . ?
O4 C6 O4 C7 1.8(13) 12_565 . . . ?
C5 C6 O4 C7 -175.4(8) . . . . ?
C7 C7 O4 C6 -175.2(12) 5_675 . . . ?
_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.122
_refine_diff_density_min -0.404
_refine_diff_density_rms 0.098
Notice: (null)(): Re-Authentication Failure (errflg=1) in Unknown on line 0