 
data_natromarkeyite
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_mineral            'markeyite' 
_chemical_compound_source         'Markey mine, Utah'
_chemical_formula_sum
 'C13 H54 Ca8 Na2 O74 U4' 
_chemical_formula_weight          2713.30

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'
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na'  'Na'   0.0362   0.0249
 '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'
 'U'  'U'  -9.6767   9.6646
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            59
_space_group_name_H-M_alt         'P m m n'
_space_group_name_Hall            '-P 2ab 2a'
 
_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+1/2, y, z'
 'x, -y+1/2, z'
 '-x+1/2, -y+1/2, z'
 '-x, -y, -z'
 'x-1/2, -y, -z'
 '-x, y-1/2, -z'
 'x-1/2, y-1/2, -z'
 
_cell_length_a                    17.8820(13)
_cell_length_b                    18.3030(4)
_cell_length_c                    10.2249(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3346.6(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     17496
_cell_measurement_theta_min       3.0
_cell_measurement_theta_max       25.0
_exptl_crystal_density_diffrn     2.693          
_exptl_crystal_F_000              2548
_exptl_crystal_size_max           0.100
_exptl_crystal_size_mid           0.100
_exptl_crystal_size_min           0.030
_exptl_absorpt_coefficient_mu     10.419
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    Higashi2001 
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_correction_T_min   0.597
_exptl_crystal_description        'Tablet'
_exptl_crystal_colour             'Yellow'
_shelx_estimated_absorpt_T_min    0.422
_shelx_estimated_absorpt_T_max    0.745
_diffrn_measurement_device_type   'Rigaku R-axis RAPID II'
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71075
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_radiation_monochromator   graphite 
_diffrn_reflns_number             20715
_diffrn_reflns_av_unetI/netI      0.0213
_diffrn_reflns_av_R_equivalents   0.0343
_diffrn_reflns_limit_h_min        -21
_diffrn_reflns_limit_h_max        21
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.197
_diffrn_reflns_theta_max          25.026
_diffrn_reflns_theta_full         25.026
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  0.994
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   0.994
_diffrn_reflns_point_group_measured_fraction_max   0.994
_diffrn_reflns_point_group_measured_fraction_full  0.994
_reflns_number_total              3150
_reflns_number_gt                 2898
_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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0201P)²+9.2200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refxyz
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          3150
_refine_ls_number_parameters      309
_refine_ls_number_restraints      21
_refine_ls_R_factor_all           0.0234
_refine_ls_R_factor_gt            0.0202
_refine_ls_wR_factor_ref          0.0453
_refine_ls_wR_factor_gt           0.0442
_refine_ls_goodness_of_fit_ref    1.045
_refine_ls_restrained_S_all       1.043
_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
U1 U 0.46930(2) 0.750000 0.99124(2) 0.01533(7) Uani 1 2 d S T P . .
U2 U 0.250000 0.46718(2) 0.07581(2) 0.01935(7) Uani 1 2 d S T P . .
Ca1 Ca 0.44003(4) 0.43571(4) 0.87349(8) 0.01445(17) Uani 1 1 d . . . . .
Ca2 Ca 0.38124(5) 0.63974(5) 0.60892(8) 0.02310(19) Uani 1 1 d . . . . .
Na1 Na 0.250000 0.250000 0.6853(4) 0.0437(10) Uani 1 4 d S T P . .
Na2 Na 0.250000 0.750000 0.1043(5) 0.091(2) Uani 1 4 d S T P . .
C1 C 0.4269(2) 0.6130(2) 0.8739(4) 0.0177(8) Uani 1 1 d . . . . .
C2 C 0.6095(2) 0.4928(2) 0.8074(4) 0.0205(9) Uani 1 1 d . . . . .
C3 C 0.250000 0.4033(3) 0.8191(6) 0.0234(13) Uani 1 2 d S T P . .
C4 C 0.4388(4) 0.250000 0.7774(7) 0.0357(17) Uani 1 2 d S T P . .
C5 C 0.250000 0.7232(6) 0.5850(12) 0.023(3) Uani 0.5 2 d S T P . .
O1 O 0.40941(15) 0.55646(14) 0.8130(3) 0.0215(6) Uani 1 1 d . . . . .
O2 O 0.46666(15) 0.61501(15) 0.9792(3) 0.0227(7) Uani 1 1 d . . . . .
O3 O 0.40536(17) 0.67674(14) 0.8303(3) 0.0250(7) Uani 1 1 d . . . . .
O4 O 0.55004(14) 0.46709(15) 0.7591(3) 0.0227(6) Uani 1 1 d . . . . .
O5 O 0.67282(15) 0.48721(18) 0.7470(3) 0.0306(7) Uani 1 1 d . . . . .
O6 O 0.38786(15) 0.47324(16) 0.0820(3) 0.0236(7) Uani 1 1 d . . . . .
O7 O 0.250000 0.3766(2) 0.7067(4) 0.0310(10) Uani 1 2 d S T P . .
O8 O 0.31061(15) 0.41739(18) 0.8838(3) 0.0289(7) Uani 1 1 d . . . . .
O9 O 0.4025(4) 0.250000 0.6754(6) 0.082(3) Uani 1 2 d S T P . .
O10 O 0.46009(18) 0.30954(15) 0.8378(3) 0.0309(8) Uani 1 1 d . . . . .
O11 O 0.3875(2) 0.750000 0.0924(4) 0.0287(10) Uani 1 2 d S T P . .
O12 O 0.5497(2) 0.750000 0.8901(5) 0.0336(11) Uani 1 2 d S T P . .
O13 O 0.250000 0.3783(2) 0.1463(5) 0.0340(11) Uani 1 2 d S T P . .
O14 O 0.250000 0.5567(2) 0.0074(4) 0.0313(10) Uani 1 2 d S T P . .
O15 O 0.3132(2) 0.750000 0.5731(5) 0.0292(10) Uani 1 2 d S T P . .
O16 O 0.250000 0.6545(5) 0.6237(10) 0.034(2) Uani 0.5 2 d S T P . .
OW1 O 0.3291(2) 0.52893(18) 0.5187(3) 0.0351(8) Uani 1 1 d D . . . .
H1A H 0.328(3) 0.526(3) 0.4379(19) 0.042 Uiso 1 1 d D U . . .
H1B H 0.360(2) 0.499(2) 0.539(4) 0.042 Uiso 1 1 d D U . . .
OW2 O 0.40387(18) 0.41062(18) 0.6402(3) 0.0337(8) Uani 1 1 d D . . . .
H2A H 0.395(2) 0.3682(10) 0.635(5) 0.040 Uiso 1 1 d D U . . .
H2B H 0.3675(18) 0.433(2) 0.620(5) 0.040 Uiso 1 1 d D U . . .
OW3 O 0.250000 0.6651(3) 0.2660(7) 0.0655(18) Uani 1 2 d DS T P . .
H3A H 0.250000 0.6212(11) 0.267(7) 0.079 Uiso 1 2 d DS U P . .
H3B H 0.250000 0.680(4) 0.340(4) 0.079 Uiso 1 2 d DS U P . .
OW4 O 0.4013(2) 0.6617(2) 0.3763(3) 0.0417(9) Uani 1 1 d D . . . .
H4A H 0.416(3) 0.629(2) 0.330(4) 0.050 Uiso 1 1 d D U . . .
H4B H 0.3633(19) 0.677(3) 0.344(5) 0.050 Uiso 1 1 d D U . . .
OW5 O 0.4764(3) 0.750000 0.5880(6) 0.0415(12) Uani 1 2 d DS T P . .
H5A H 0.495(4) 0.750000 0.514(3) 0.050 Uiso 1 2 d DS U P . .
H5B H 0.509(4) 0.728(5) 0.631(6) 0.050 Uiso 0.5 1 d D U P . .
OW6 O 0.4995(2) 0.5811(2) 0.5816(4) 0.0484(10) Uani 1 1 d D . . . .
H6A H 0.513(3) 0.5426(17) 0.614(6) 0.058 Uiso 1 1 d D U . . .
H6B H 0.535(2) 0.607(2) 0.578(6) 0.058 Uiso 1 1 d D U . . .
OW7 O 0.250000 0.6247(4) 0.7372(8) 0.0192(17) Uani 0.5 2 d DS T P . .
H7A H 0.250000 0.660(3) 0.787(7) 0.023 Uiso 0.5 2 d DS U P . .
H7B H 0.250000 0.588(3) 0.783(8) 0.023 Uiso 0.5 2 d DS U P . .
OW8 O 0.250000 0.750000 0.8832(7) 0.0428(18) Uani 1 4 d S T P . .
OW9 O 0.250000 0.250000 0.9275(10) 0.115(5) Uani 1 4 d S T P . .
OW10 O 0.6288(5) 0.6751(6) 0.6665(9) 0.154(6) Uani 0.797(19) 1 d . . P . .
OW11 O 0.250000 0.250000 0.4693(14) 0.213(16) Uani 0.96(5) 4 d S T P . .
 
 
_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
U1 O12 1.771(4) . ?
U1 O11 1.791(4) 1_556 ?
U1 O3 2.411(3) 3_565 ?
U1 O3 2.411(3) . ?
U1 O10 2.416(3) 7_667 ?
U1 O10 2.416(3) 5_667 ?
U1 O2 2.474(3) 3_565 ?
U1 O2 2.474(3) . ?
U1 C4 2.881(6) 5_667 ?
U1 C1 2.882(4) . ?
U1 C1 2.882(4) 3_565 ?
U1 Ca1 4.0118(7) 7_667 ?
U2 O13 1.779(4) . ?
U2 O14 1.782(4) . ?
U2 O8 2.420(3) 2_554 ?
U2 O8 2.420(3) 1_554 ?
U2 O5 2.426(3) 5_666 ?
U2 O5 2.426(3) 6_566 ?
U2 O6 2.469(3) . ?
U2 O6 2.469(3) 2 ?
U2 C3 2.873(6) 1_554 ?
U2 C2 2.877(4) 5_666 ?
U2 C2 2.877(4) 6_566 ?
U2 Ca1 4.0198(8) 2_554 ?
Ca1 O8 2.341(3) . ?
Ca1 O1 2.359(3) . ?
Ca1 O4 2.360(3) . ?
Ca1 O10 2.365(3) . ?
Ca1 O6 2.426(3) 1_556 ?
Ca1 O2 2.432(3) 5_667 ?
Ca1 OW2 2.514(3) . ?
Ca1 Ca1 4.1026(15) 5_667 ?
Ca2 O16 2.3671(15) . ?
Ca2 O15 2.385(2) . ?
Ca2 OW6 2.389(3) . ?
Ca2 O3 2.402(3) . ?
Ca2 OW1 2.416(3) . ?
Ca2 OW4 2.439(4) . ?
Ca2 O1 2.633(3) . ?
Ca2 OW5 2.649(3) . ?
Ca2 OW7 2.702(4) . ?
Ca2 C5 2.811(6) . ?
Ca2 C1 2.871(4) . ?
Ca2 Ca2 4.0362(17) 3_565 ?
Ca2 H1B 2.70(5) . ?
Na1 OW11 2.208(15) . ?
Na1 O7 2.327(5) . ?
Na1 O7 2.327(5) 3 ?
Na1 OW9 2.477(11) . ?
Na1 O9 2.729(8) 2 ?
Na1 O9 2.729(8) . ?
Na1 C3 3.122(6) 3 ?
Na1 C3 3.122(6) . ?
Na2 OW8 2.261(9) 1_554 ?
Na2 OW3 2.269(7) . ?
Na2 OW3 2.269(7) 3_565 ?
Na2 O11 2.462(4) 2 ?
Na2 O11 2.462(4) . ?
C1 O1 1.247(5) . ?
C1 O2 1.292(5) . ?
C1 O3 1.306(5) . ?
C2 O4 1.263(5) . ?
C2 O6 1.291(5) 5_666 ?
C2 O5 1.294(5) . ?
C3 O7 1.249(7) . ?
C3 O8 1.296(4) . ?
C3 O8 1.296(4) 2 ?
C4 O9 1.228(8) . ?
C4 O10 1.309(4) . ?
C4 O10 1.309(4) 3 ?
C5 C5 0.98(2) 3_565 ?
C5 O15 1.238(6) . ?
C5 O15 1.238(6) 2 ?
C5 O16 1.319(14) . ?
O12 OW10 3.018(11) . ?
O16 OW7 1.282(12) . ?
O16 OW8 3.177(11) . ?
OW1 H1A 0.828(19) . ?
OW1 H1B 0.811(19) . ?
OW2 H2A 0.794(19) . ?
OW2 H2B 0.792(19) . ?
OW3 H3A 0.80(2) . ?
OW3 H3B 0.81(2) . ?
OW4 H4A 0.805(19) . ?
OW4 H4B 0.806(19) . ?
OW5 H5A 0.83(2) . ?
OW5 H5B 0.83(2) . ?
OW5 H5B 0.83(2) 3_565 ?
OW6 H6A 0.814(19) . ?
OW6 H6B 0.797(19) . ?
OW7 H7A 0.82(2) . ?
OW7 H7B 0.81(2) . ?
 
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
O12 U1 O11 179.5(2) . 1_556 ?
O12 U1 O3 89.24(15) . 3_565 ?
O11 U1 O3 90.39(14) 1_556 3_565 ?
O12 U1 O3 89.24(15) . . ?
O11 U1 O3 90.39(14) 1_556 . ?
O3 U1 O3 67.58(12) 3_565 . ?
O12 U1 O10 89.89(16) . 7_667 ?
O11 U1 O10 90.51(15) 1_556 7_667 ?
O3 U1 O10 119.39(9) 3_565 7_667 ?
O3 U1 O10 172.96(9) . 7_667 ?
O12 U1 O10 89.89(16) . 5_667 ?
O11 U1 O10 90.51(15) 1_556 5_667 ?
O3 U1 O10 172.96(9) 3_565 5_667 ?
O3 U1 O10 119.39(9) . 5_667 ?
O10 U1 O10 53.62(13) 7_667 5_667 ?
O12 U1 O2 89.23(7) . 3_565 ?
O11 U1 O2 90.75(7) 1_556 3_565 ?
O3 U1 O2 53.25(9) 3_565 3_565 ?
O3 U1 O2 120.83(9) . 3_565 ?
O10 U1 O2 66.14(9) 7_667 3_565 ?
O10 U1 O2 119.75(9) 5_667 3_565 ?
O12 U1 O2 89.23(7) . . ?
O11 U1 O2 90.75(7) 1_556 . ?
O3 U1 O2 120.83(9) 3_565 . ?
O3 U1 O2 53.26(9) . . ?
O10 U1 O2 119.75(9) 7_667 . ?
O10 U1 O2 66.13(9) 5_667 . ?
O2 U1 O2 173.91(13) 3_565 . ?
O12 U1 C4 90.9(2) . 5_667 ?
O11 U1 C4 89.5(2) 1_556 5_667 ?
O3 U1 C4 146.21(6) 3_565 5_667 ?
O3 U1 C4 146.21(6) . 5_667 ?
O10 U1 C4 26.83(6) 7_667 5_667 ?
O10 U1 C4 26.83(7) 5_667 5_667 ?
O2 U1 C4 92.96(6) 3_565 5_667 ?
O2 U1 C4 92.96(6) . 5_667 ?
O12 U1 C1 88.32(11) . . ?
O11 U1 C1 91.45(11) 1_556 . ?
O3 U1 C1 94.29(10) 3_565 . ?
O3 U1 C1 26.73(10) . . ?
O10 U1 C1 146.25(10) 7_667 . ?
O10 U1 C1 92.67(10) 5_667 . ?
O2 U1 C1 147.48(10) 3_565 . ?
O2 U1 C1 26.55(10) . . ?
C4 U1 C1 119.50(8) 5_667 . ?
O12 U1 C1 88.32(11) . 3_565 ?
O11 U1 C1 91.45(10) 1_556 3_565 ?
O3 U1 C1 26.73(10) 3_565 3_565 ?
O3 U1 C1 94.29(10) . 3_565 ?
O10 U1 C1 92.67(10) 7_667 3_565 ?
O10 U1 C1 146.25(10) 5_667 3_565 ?
O2 U1 C1 26.55(10) 3_565 3_565 ?
O2 U1 C1 147.48(10) . 3_565 ?
C4 U1 C1 119.50(8) 5_667 3_565 ?
C1 U1 C1 120.95(16) . 3_565 ?
O12 U1 Ca1 82.71(8) . 7_667 ?
O11 U1 Ca1 97.52(7) 1_556 7_667 ?
O3 U1 Ca1 87.46(6) 3_565 7_667 ?
O3 U1 Ca1 153.92(6) . 7_667 ?
O10 U1 Ca1 32.57(7) 7_667 7_667 ?
O10 U1 Ca1 85.50(7) 5_667 7_667 ?
O2 U1 Ca1 34.79(6) 3_565 7_667 ?
O2 U1 Ca1 150.56(6) . 7_667 ?
C4 U1 Ca1 59.09(3) 5_667 7_667 ?
C1 U1 Ca1 170.85(8) . 7_667 ?
C1 U1 Ca1 60.85(8) 3_565 7_667 ?
O13 U2 O14 179.2(2) . . ?
O13 U2 O8 89.09(16) . 2_554 ?
O14 U2 O8 91.60(15) . 2_554 ?
O13 U2 O8 89.09(16) . 1_554 ?
O14 U2 O8 91.60(15) . 1_554 ?
O8 U2 O8 53.21(13) 2_554 1_554 ?
O13 U2 O5 90.70(15) . 5_666 ?
O14 U2 O5 88.66(14) . 5_666 ?
O8 U2 O5 171.93(9) 2_554 5_666 ?
O8 U2 O5 118.72(9) 1_554 5_666 ?
O13 U2 O5 90.70(15) . 6_566 ?
O14 U2 O5 88.66(14) . 6_566 ?
O8 U2 O5 118.72(9) 2_554 6_566 ?
O8 U2 O5 171.93(9) 1_554 6_566 ?
O5 U2 O5 69.34(13) 5_666 6_566 ?
O13 U2 O6 91.76(7) . . ?
O14 U2 O6 88.20(7) . . ?
O8 U2 O6 119.01(9) 2_554 . ?
O8 U2 O6 65.82(9) 1_554 . ?
O5 U2 O6 52.94(9) 5_666 . ?
O5 U2 O6 122.24(9) 6_566 . ?
O13 U2 O6 91.76(7) . 2 ?
O14 U2 O6 88.20(7) . 2 ?
O8 U2 O6 65.82(9) 2_554 2 ?
O8 U2 O6 119.01(9) 1_554 2 ?
O5 U2 O6 122.24(9) 5_666 2 ?
O5 U2 O6 52.94(9) 6_566 2 ?
O6 U2 O6 174.07(13) . 2 ?
O13 U2 C3 89.9(2) . 1_554 ?
O14 U2 C3 90.89(19) . 1_554 ?
O8 U2 C3 26.62(6) 2_554 1_554 ?
O8 U2 C3 26.62(6) 1_554 1_554 ?
O5 U2 C3 145.32(6) 5_666 1_554 ?
O5 U2 C3 145.32(6) 6_566 1_554 ?
O6 U2 C3 92.39(6) . 1_554 ?
O6 U2 C3 92.39(6) 2 1_554 ?
O13 U2 C2 93.71(11) . 5_666 ?
O14 U2 C2 85.91(11) . 5_666 ?
O8 U2 C2 145.45(10) 2_554 5_666 ?
O8 U2 C2 92.37(10) 1_554 5_666 ?
O5 U2 C2 26.55(10) 5_666 5_666 ?
O5 U2 C2 95.69(10) 6_566 5_666 ?
O6 U2 C2 26.58(10) . 5_666 ?
O6 U2 C2 148.23(11) 2 5_666 ?
C3 U2 C2 118.86(8) 1_554 5_666 ?
O13 U2 C2 93.71(11) . 6_566 ?
O14 U2 C2 85.91(11) . 6_566 ?
O8 U2 C2 92.37(10) 2_554 6_566 ?
O8 U2 C2 145.45(10) 1_554 6_566 ?
O5 U2 C2 95.69(10) 5_666 6_566 ?
O5 U2 C2 26.55(10) 6_566 6_566 ?
O6 U2 C2 148.23(11) . 6_566 ?
O6 U2 C2 26.58(10) 2 6_566 ?
C3 U2 C2 118.86(8) 1_554 6_566 ?
C2 U2 C2 121.72(16) 5_666 6_566 ?
O13 U2 Ca1 94.44(9) . 2_554 ?
O14 U2 Ca1 85.97(8) . 2_554 ?
O8 U2 Ca1 31.80(7) 2_554 2_554 ?
O8 U2 Ca1 84.68(7) 1_554 2_554 ?
O5 U2 Ca1 156.15(7) 5_666 2_554 ?
O5 U2 Ca1 87.29(7) 6_566 2_554 ?
O6 U2 Ca1 149.75(7) . 2_554 ?
O6 U2 Ca1 34.45(6) 2 2_554 ?
C3 U2 Ca1 58.103(16) 1_554 2_554 ?
C2 U2 Ca1 171.29(8) 5_666 2_554 ?
C2 U2 Ca1 60.77(8) 6_566 2_554 ?
O8 Ca1 O1 85.21(11) . . ?
O8 Ca1 O4 151.83(11) . . ?
O1 Ca1 O4 80.54(10) . . ?
O8 Ca1 O10 90.98(11) . . ?
O1 Ca1 O10 155.40(11) . . ?
O4 Ca1 O10 91.99(11) . . ?
O8 Ca1 O6 67.71(10) . 1_556 ?
O1 Ca1 O6 82.87(10) . 1_556 ?
O4 Ca1 O6 133.40(10) . 1_556 ?
O10 Ca1 O6 118.06(11) . 1_556 ?
O8 Ca1 O2 126.57(11) . 5_667 ?
O1 Ca1 O2 132.78(10) . 5_667 ?
O4 Ca1 O2 80.08(10) . 5_667 ?
O10 Ca1 O2 67.59(10) . 5_667 ?
O6 Ca1 O2 80.09(10) 1_556 5_667 ?
O8 Ca1 OW2 76.26(11) . . ?
O1 Ca1 OW2 82.11(10) . . ?
O4 Ca1 OW2 77.79(11) . . ?
O10 Ca1 OW2 73.39(11) . . ?
O6 Ca1 OW2 141.87(11) 1_556 . ?
O2 Ca1 OW2 133.97(11) 5_667 . ?
O8 Ca1 U1 105.23(8) . 5_667 ?
O1 Ca1 U1 167.90(7) . 5_667 ?
O4 Ca1 U1 92.30(7) . 5_667 ?
O10 Ca1 U1 33.36(7) . 5_667 ?
O6 Ca1 U1 95.30(7) 1_556 5_667 ?
O2 Ca1 U1 35.49(6) 5_667 5_667 ?
OW2 Ca1 U1 106.04(8) . 5_667 ?
O8 Ca1 U2 33.02(7) . 1_556 ?
O1 Ca1 U2 78.73(7) . 1_556 ?
O4 Ca1 U2 157.67(7) . 1_556 ?
O10 Ca1 U2 110.34(9) . 1_556 ?
O6 Ca1 U2 35.14(7) 1_556 1_556 ?
O2 Ca1 U2 108.43(7) 5_667 1_556 ?
OW2 Ca1 U2 107.29(8) . 1_556 ?
U1 Ca1 U2 106.596(18) 5_667 1_556 ?
O8 Ca1 Ca1 124.79(8) . 5_667 ?
O1 Ca1 Ca1 75.48(7) . 5_667 ?
O4 Ca1 Ca1 74.75(7) . 5_667 ?
O10 Ca1 Ca1 125.32(8) . 5_667 ?
O6 Ca1 Ca1 58.97(7) 1_556 5_667 ?
O2 Ca1 Ca1 57.98(7) 5_667 5_667 ?
OW2 Ca1 Ca1 146.89(8) . 5_667 ?
U1 Ca1 Ca1 93.29(2) 5_667 5_667 ?
U2 Ca1 Ca1 92.02(2) 1_556 5_667 ?
O16 Ca2 O15 53.7(2) . . ?
O16 Ca2 OW6 159.5(2) . . ?
O15 Ca2 OW6 144.52(14) . . ?
O16 Ca2 O3 94.9(3) . . ?
O15 Ca2 O3 89.86(13) . . ?
OW6 Ca2 O3 94.48(13) . . ?
O16 Ca2 OW1 74.8(2) . . ?
O15 Ca2 OW1 117.05(13) . . ?
OW6 Ca2 OW1 85.40(14) . . ?
O3 Ca2 OW1 131.77(11) . . ?
O16 Ca2 OW4 100.9(3) . . ?
O15 Ca2 OW4 77.64(14) . . ?
OW6 Ca2 OW4 80.18(13) . . ?
O3 Ca2 OW4 147.80(12) . . ?
OW1 Ca2 OW4 79.79(12) . . ?
O16 Ca2 O1 101.8(2) . . ?
O15 Ca2 O1 135.17(13) . . ?
OW6 Ca2 O1 70.31(11) . . ?
O3 Ca2 O1 51.82(8) . . ?
OW1 Ca2 O1 83.72(10) . . ?
OW4 Ca2 O1 147.16(11) . . ?
O16 Ca2 OW5 123.7(2) . . ?
O15 Ca2 OW5 70.78(12) . . ?
OW6 Ca2 OW5 76.35(13) . . ?
O3 Ca2 OW5 75.27(14) . . ?
OW1 Ca2 OW5 148.99(14) . . ?
OW4 Ca2 OW5 72.60(15) . . ?
O1 Ca2 OW5 112.46(13) . . ?
O16 Ca2 OW7 28.3(3) . . ?
O15 Ca2 OW7 73.60(18) . . ?
OW6 Ca2 OW7 141.26(18) . . ?
O3 Ca2 OW7 74.17(17) . . ?
OW1 Ca2 OW7 76.38(18) . . ?
OW4 Ca2 OW7 128.18(17) . . ?
O1 Ca2 OW7 73.89(16) . . ?
OW5 Ca2 OW7 132.44(19) . . ?
O16 Ca2 C5 27.9(3) . . ?
O15 Ca2 C5 25.9(2) . . ?
OW6 Ca2 C5 166.8(3) . . ?
O3 Ca2 C5 94.5(3) . . ?
OW1 Ca2 C5 95.8(2) . . ?
OW4 Ca2 C5 87.1(3) . . ?
O1 Ca2 C5 122.9(2) . . ?
OW5 Ca2 C5 96.6(2) . . ?
OW7 Ca2 C5 51.1(3) . . ?
O16 Ca2 C1 103.9(3) . . ?
O15 Ca2 C1 115.72(13) . . ?
OW6 Ca2 C1 77.43(13) . . ?
O3 Ca2 C1 26.85(10) . . ?
OW1 Ca2 C1 109.10(11) . . ?
OW4 Ca2 C1 155.01(12) . . ?
O1 Ca2 C1 25.73(9) . . ?
OW5 Ca2 C1 91.34(15) . . ?
OW7 Ca2 C1 76.79(17) . . ?
C5 Ca2 C1 114.3(3) . . ?
O16 Ca2 Ca2 83.5(2) . 3_565 ?
O15 Ca2 Ca2 32.19(9) . 3_565 ?
OW6 Ca2 Ca2 116.72(11) . 3_565 ?
O3 Ca2 Ca2 73.62(6) . 3_565 ?
OW1 Ca2 Ca2 147.09(8) . 3_565 ?
OW4 Ca2 Ca2 80.51(9) . 3_565 ?
O1 Ca2 Ca2 125.38(6) . 3_565 ?
OW5 Ca2 Ca2 40.37(8) . 3_565 ?
OW7 Ca2 Ca2 95.84(16) . 3_565 ?
C5 Ca2 Ca2 57.08(19) . 3_565 ?
C1 Ca2 Ca2 99.81(7) . 3_565 ?
O16 Ca2 H1B 89.3(8) . . ?
O15 Ca2 H1B 134.1(6) . . ?
OW6 Ca2 H1B 70.4(8) . . ?
O3 Ca2 H1B 122.9(8) . . ?
OW1 Ca2 H1B 17.1(6) . . ?
OW4 Ca2 H1B 85.5(9) . . ?
O1 Ca2 H1B 71.5(7) . . ?
OW5 Ca2 H1B 142.7(10) . . ?
OW7 Ca2 H1B 84.8(10) . . ?
C5 Ca2 H1B 112.3(7) . . ?
C1 Ca2 H1B 97.2(7) . . ?
Ca2 Ca2 H1B 162.6(7) 3_565 . ?
OW11 Na1 O7 95.40(16) . . ?
OW11 Na1 O7 95.40(16) . 3 ?
O7 Na1 O7 169.2(3) . 3 ?
OW11 Na1 OW9 180.0 . . ?
O7 Na1 OW9 84.60(16) . . ?
O7 Na1 OW9 84.60(16) 3 . ?
OW11 Na1 O9 87.88(16) . 2 ?
O7 Na1 O9 90.199(14) . 2 ?
O7 Na1 O9 90.199(14) 3 2 ?
OW9 Na1 O9 92.12(16) . 2 ?
OW11 Na1 O9 87.88(16) . . ?
O7 Na1 O9 90.199(14) . . ?
O7 Na1 O9 90.200(14) 3 . ?
OW9 Na1 O9 92.12(16) . . ?
O9 Na1 O9 175.8(3) 2 . ?
OW11 Na1 C3 116.00(14) . 3 ?
O7 Na1 C3 148.6(2) . 3 ?
O7 Na1 C3 20.60(16) 3 3 ?
OW9 Na1 C3 64.00(14) . 3 ?
O9 Na1 C3 90.93(7) 2 3 ?
O9 Na1 C3 90.93(7) . 3 ?
OW11 Na1 C3 116.00(14) . . ?
O7 Na1 C3 20.60(16) . . ?
O7 Na1 C3 148.6(2) 3 . ?
OW9 Na1 C3 64.00(14) . . ?
O9 Na1 C3 90.93(7) 2 . ?
O9 Na1 C3 90.93(7) . . ?
C3 Na1 C3 128.0(3) 3 . ?
OW8 Na2 OW3 136.79(18) 1_554 . ?
OW8 Na2 OW3 136.79(18) 1_554 3_565 ?
OW3 Na2 OW3 86.4(4) . 3_565 ?
OW8 Na2 O11 87.17(15) 1_554 2 ?
OW3 Na2 O11 92.06(11) . 2 ?
OW3 Na2 O11 92.06(11) 3_565 2 ?
OW8 Na2 O11 87.17(15) 1_554 . ?
OW3 Na2 O11 92.06(11) . . ?
OW3 Na2 O11 92.06(11) 3_565 . ?
O11 Na2 O11 174.3(3) 2 . ?
OW8 Na2 U1 73.58(7) 1_554 2_554 ?
OW3 Na2 U1 101.89(4) . 2_554 ?
OW3 Na2 U1 101.89(4) 3_565 2_554 ?
O11 Na2 U1 13.59(11) 2 2_554 ?
O11 Na2 U1 160.7(2) . 2_554 ?
OW8 Na2 U1 73.58(7) 1_554 1_554 ?
OW3 Na2 U1 101.89(4) . 1_554 ?
OW3 Na2 U1 101.89(4) 3_565 1_554 ?
O11 Na2 U1 160.7(2) 2 1_554 ?
O11 Na2 U1 13.59(11) . 1_554 ?
U1 Na2 U1 147.16(13) 2_554 1_554 ?
O1 C1 O2 125.3(4) . . ?
O1 C1 O3 119.8(4) . . ?
O2 C1 O3 114.9(3) . . ?
O1 C1 Ca2 66.4(2) . . ?
O2 C1 Ca2 159.8(3) . . ?
O3 C1 Ca2 56.14(19) . . ?
O1 C1 U1 174.7(3) . . ?
O2 C1 U1 58.85(19) . . ?
O3 C1 U1 56.11(18) . . ?
Ca2 C1 U1 108.64(12) . . ?
O4 C2 O6 123.6(4) . 5_666 ?
O4 C2 O5 121.3(4) . . ?
O6 C2 O5 115.1(3) 5_666 . ?
O4 C2 U2 172.9(3) . 5_666 ?
O6 C2 U2 58.80(19) 5_666 5_666 ?
O5 C2 U2 56.9(2) . 5_666 ?
O7 C3 O8 123.2(3) . . ?
O7 C3 O8 123.2(3) . 2 ?
O8 C3 O8 113.5(5) . 2 ?
O7 C3 U2 179.0(5) . 1_556 ?
O8 C3 U2 56.8(3) . 1_556 ?
O8 C3 U2 56.8(3) 2 1_556 ?
O7 C3 Na1 40.9(3) . . ?
O8 C3 Na1 113.7(3) . . ?
O8 C3 Na1 113.7(3) 2 . ?
U2 C3 Na1 140.0(2) 1_556 . ?
O9 C4 O10 123.7(3) . . ?
O9 C4 O10 123.7(3) . 3 ?
O10 C4 O10 112.7(5) . 3 ?
O9 C4 U1 177.1(7) . 5_667 ?
O10 C4 U1 56.4(3) . 5_667 ?
O10 C4 U1 56.4(3) 3 5_667 ?
C5 C5 O15 66.6(5) 3_565 . ?
C5 C5 O15 66.6(5) 3_565 2 ?
O15 C5 O15 131.8(10) . 2 ?
C5 C5 O16 162.5(7) 3_565 . ?
O15 C5 O16 114.0(5) . . ?
O15 C5 O16 114.0(5) 2 . ?
C5 C5 Ca2 122.92(19) 3_565 2 ?
O15 C5 Ca2 170.4(7) . 2 ?
O15 C5 Ca2 57.4(3) 2 2 ?
O16 C5 Ca2 57.0(2) . 2 ?
C5 C5 Ca2 122.92(19) 3_565 . ?
O15 C5 Ca2 57.4(3) . . ?
O15 C5 Ca2 170.4(7) 2 . ?
O16 C5 Ca2 57.0(2) . . ?
Ca2 C5 Ca2 113.2(4) 2 . ?
C1 O1 Ca1 126.1(3) . . ?
C1 O1 Ca2 87.9(2) . . ?
Ca1 O1 Ca2 142.61(12) . . ?
C1 O2 Ca1 152.1(2) . 5_667 ?
C1 O2 U1 94.6(2) . . ?
Ca1 O2 U1 109.72(10) 5_667 . ?
C1 O3 Ca2 97.0(2) . . ?
C1 O3 U1 97.2(2) . . ?
Ca2 O3 U1 152.27(14) . . ?
C2 O4 Ca1 126.8(3) . . ?
C2 O5 U2 96.5(2) . 5_666 ?
C2 O6 Ca1 153.1(3) 5_666 1_554 ?
C2 O6 U2 94.6(2) 5_666 . ?
Ca1 O6 U2 110.41(11) 1_554 . ?
C3 O7 Na1 118.5(4) . . ?
C3 O8 Ca1 146.3(3) . . ?
C3 O8 U2 96.6(3) . 1_556 ?
Ca1 O8 U2 115.18(12) . 1_556 ?
C4 O9 Na1 119.7(6) . . ?
C4 O10 Ca1 147.3(3) . . ?
C4 O10 U1 96.8(3) . 5_667 ?
Ca1 O10 U1 114.08(12) . 5_667 ?
U1 O11 Na2 147.6(3) 1_554 . ?
U1 O12 OW10 145.4(2) . . ?
C5 O15 C5 46.7(10) 3_565 . ?
C5 O15 Ca2 96.6(5) 3_565 3_565 ?
C5 O15 Ca2 141.8(5) . 3_565 ?
C5 O15 Ca2 141.8(5) 3_565 . ?
C5 O15 Ca2 96.6(5) . . ?
Ca2 O15 Ca2 115.62(17) 3_565 . ?
OW7 O16 C5 132.6(10) . . ?
OW7 O16 Ca2 90.5(2) . 2 ?
C5 O16 Ca2 95.1(2) . 2 ?
OW7 O16 Ca2 90.5(2) . . ?
C5 O16 Ca2 95.1(2) . . ?
Ca2 O16 Ca2 165.0(4) 2 . ?
OW7 O16 OW8 58.5(5) . . ?
C5 O16 OW8 74.1(7) . . ?
Ca2 O16 OW8 96.7(2) 2 . ?
Ca2 O16 OW8 96.7(2) . . ?
Ca2 OW1 H1A 117(4) . . ?
Ca2 OW1 H1B 102(4) . . ?
H1A OW1 H1B 103(3) . . ?
Ca1 OW2 H2A 107(4) . . ?
Ca1 OW2 H2B 111(4) . . ?
H2A OW2 H2B 109(3) . . ?
Na2 OW3 H3A 134(6) . . ?
Na2 OW3 H3B 117(6) . . ?
H3A OW3 H3B 109(4) . . ?
Ca2 OW4 H4A 120(4) . . ?
Ca2 OW4 H4B 109(4) . . ?
H4A OW4 H4B 108(3) . . ?
Ca2 OW5 Ca2 99.26(16) . 3_565 ?
Ca2 OW5 H5A 109(3) . . ?
Ca2 OW5 H5A 109(3) 3_565 . ?
Ca2 OW5 H5B 92(6) . . ?
Ca2 OW5 H5B 140(6) 3_565 . ?
H5A OW5 H5B 103(3) . . ?
Ca2 OW5 H5B 140(6) . 3_565 ?
Ca2 OW5 H5B 92(6) 3_565 3_565 ?
H5A OW5 H5B 103(3) . 3_565 ?
H5B OW5 H5B 58(10) . 3_565 ?
Ca2 OW6 H6A 127(4) . . ?
Ca2 OW6 H6B 117(4) . . ?
H6A OW6 H6B 108(3) . . ?
O16 OW7 Ca2 61.14(16) . 2 ?
O16 OW7 Ca2 61.14(16) . . ?
Ca2 OW7 Ca2 120.5(3) 2 . ?
O16 OW7 H7A 104(7) . . ?
Ca2 OW7 H7A 103(3) 2 . ?
Ca2 OW7 H7A 103(3) . . ?
O16 OW7 H7B 150(7) . . ?
Ca2 OW7 H7B 111(2) 2 . ?
Ca2 OW7 H7B 111(2) . . ?
H7A OW7 H7B 106(4) . . ?
Na2 OW8 O16 146.61(18) 1_556 . ?
Na2 OW8 O11 48.98(12) 1_556 1_556 ?
O16 OW8 O11 123.23(10) . 1_556 ?
Na1 OW9 O13 133.60(15) . 1_556 ?
O12 OW10 O13 90.2(3) . 5_666 ?
Na1 OW11 OW10 118.4(3) . 5_666 ?
 
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 
OW1 H1A O5  0.828(19) 1.90(2) 2.732(4) 176(5) 5_666
OW2 H2A O9  0.794(19) 2.21(2) 2.962(3) 159(5) .
OW2 H2B O7  0.792(19) 2.50(5) 2.902(4) 113(4) .
OW2 H2B OW1  0.792(19) 2.16(3) 2.832(5) 143(5) .
OW3 H3A O5  0.80(2) 2.422(17) 3.114(6) 144.9(10) 5_666
OW3 H3A O5  0.80(2) 2.422(17) 3.114(6) 144.9(10) 6_566
OW4 H4A O4  0.805(19) 2.07(2) 2.869(4) 170(6) 5_666
OW4 H4B OW3  0.806(19) 2.19(3) 2.933(5) 153(5) .
OW5 H5B OW10  0.83(2) 2.38(4) 3.154(10) 154(7) .
OW6 H6A O4  0.814(19) 2.13(3) 2.909(5) 159(6) .
OW6 H6B OW10  0.797(19) 2.27(3) 3.010(11) 154(6) .
OW7 H7A OW8  0.82(2) 1.92(2) 2.736(8) 172(9) .
OW7 H7B O14  0.81(2) 2.36(7) 3.030(9) 139(8) 1_556
 
_refine_diff_density_max    1.578
_refine_diff_density_min   -0.671
_refine_diff_density_rms    0.124



