data_2009src1135

#Dr. L. Martin
#There is partial disorder on some of the BEDT-TTF molecules. A few geometrical
#restraints (SADI) were used alsong with a loose global thermal restraint (SIMU).
#There is pseudo-symmetry. Although the BEDT-TTF molecules do obey this, the 
#metal oxalate sheets do not due to the subtle differences in M-O distances.

 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C37 H27 Cr N Na O14 S24'
_chemical_formula_weight          1554.03
 
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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cr'  'Cr'   0.3209   0.6236
 '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'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    10.4550(4)
_cell_length_b                    14.6532(8)
_cell_length_c                    18.1135(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.095(2)
_cell_angle_gamma                 90.00
_cell_volume                      2767.9(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6439
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Sheet
_exptl_crystal_colour             'Dark Orange'
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.865
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1574
_exptl_absorpt_coefficient_mu     1.184
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9113
_exptl_absorpt_correction_T_max   0.9883
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Parameter refinement on 22759 reflections reduced R(int) from 0.0729 to 0.0465
Ratio of minimum to maximum apparent transmission: 0.749329
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             25203
_diffrn_reflns_av_R_equivalents   0.0424
_diffrn_reflns_av_sigmaI/netI     0.0688
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          3.00
_diffrn_reflns_theta_max          27.48
_reflns_number_total              12000
_reflns_number_gt                 9431
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_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)+(0.0010P)²+12.6784P] 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_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.50(4)
_refine_ls_number_reflns          12000
_refine_ls_number_parameters      719
_refine_ls_number_restraints      279
_refine_ls_R_factor_all           0.0896
_refine_ls_R_factor_gt            0.0641
_refine_ls_wR_factor_ref          0.1360
_refine_ls_wR_factor_gt           0.1221
_refine_ls_goodness_of_fit_ref    1.088
_refine_ls_restrained_S_all       1.080
_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
Cr1 Cr 0.79829(13) 0.02612(11) 0.00750(9) 0.0234(3) Uani 1 1 d . . .
Na1 Na 0.7038(3) 0.3980(2) -0.00828(17) 0.0109(6) Uani 1 1 d . . .
C1 C 0.6013(8) 0.2199(7) 0.1812(5) 0.029(2) Uani 1 1 d U . .
H1A H 0.5816 0.2488 0.1323 0.035 Uiso 1 1 calc R . .
H1B H 0.6727 0.1766 0.1760 0.035 Uiso 1 1 calc R . .
C2 C 0.4859(9) 0.1666(7) 0.2005(5) 0.027(2) Uani 1 1 d U . .
H2A H 0.4567 0.1280 0.1578 0.032 Uiso 1 1 calc R . .
H2B H 0.4158 0.2097 0.2096 0.032 Uiso 1 1 calc R . .
C3 C 0.6016(9) 0.1664(7) 0.3410(5) 0.025(2) Uani 1 1 d U . .
C4 C 0.6583(8) 0.2449(7) 0.3272(5) 0.028(2) Uani 1 1 d U . .
C5 C 0.7237(8) 0.2101(8) 0.4659(6) 0.030(2) Uani 1 1 d U . .
C6 C 0.7805(8) 0.2098(8) 0.5344(6) 0.028(2) Uani 1 1 d U . .
C7 C 0.9031(7) 0.2556(6) 0.6570(5) 0.022(2) Uani 1 1 d U . .
C8 C 0.8477(8) 0.1742(7) 0.6716(6) 0.026(2) Uani 1 1 d U . .
C9 C 0.9127(9) 0.2034(7) 0.8227(6) 0.035(2) Uani 1 1 d U . .
H9A H 0.8421 0.2465 0.8308 0.042 Uiso 1 1 calc R . .
H9B H 0.9380 0.1739 0.8707 0.042 Uiso 1 1 calc R . .
C10 C 1.0242(8) 0.2556(7) 0.7978(5) 0.026(2) Uani 1 1 d U . .
H10A H 1.0918 0.2115 0.7865 0.032 Uiso 1 1 calc R . .
H10B H 1.0591 0.2940 0.8395 0.032 Uiso 1 1 calc R . .
S1 S 0.6554(2) 0.30642(19) 0.24483(16) 0.0354(6) Uani 1 1 d . . .
S2 S 0.5151(2) 0.09427(18) 0.28147(15) 0.0336(6) Uani 1 1 d . . .
S3 S 0.6202(2) 0.1239(2) 0.43319(14) 0.0354(7) Uani 1 1 d . . .
S4 S 0.7451(2) 0.29977(19) 0.40342(15) 0.0336(6) Uani 1 1 d . . .
S5 S 0.8817(2) 0.2997(2) 0.56816(14) 0.0332(6) Uani 1 1 d . . .
S6 S 0.7566(2) 0.12217(19) 0.59909(14) 0.0333(6) Uani 1 1 d . . .
S7 S 0.8539(2) 0.11517(19) 0.75582(16) 0.0357(7) Uani 1 1 d . . .
S8 S 0.9923(2) 0.3279(2) 0.71838(15) 0.0360(6) Uani 1 1 d . . .
C11 C 0.0116(11) 0.1037(10) 0.2063(7) 0.023(3) Uani 0.604(14) 1 d PDU A 1
H11A H -0.0185 0.1642 0.2223 0.027 Uiso 0.604(14) 1 calc PR A 1
H11B H 0.0187 0.1069 0.1522 0.027 Uiso 0.604(14) 1 calc PR A 1
C12 C -0.0910(13) 0.0343(11) 0.2207(6) 0.025(2) Uani 0.604(14) 1 d PDU A 1
H12A H -0.0583 -0.0282 0.2133 0.031 Uiso 0.604(14) 1 calc PR A 1
H12B H -0.1672 0.0440 0.1859 0.031 Uiso 0.604(14) 1 calc PR A 1
C13 C 0.0139(8) 0.0618(8) 0.3667(5) 0.033(2) Uani 1 1 d U A .
C14 C 0.1308(8) 0.0753(7) 0.3406(5) 0.025(2) Uani 1 1 d U A .
C15 C 0.1651(7) 0.0725(8) 0.4846(4) 0.029(2) Uani 1 1 d U A .
C16 C 0.2179(8) 0.0692(8) 0.5562(4) 0.027(2) Uani 1 1 d U . .
C17 C 0.3745(8) 0.0679(7) 0.6720(5) 0.029(2) Uani 1 1 d U . .
C18 C 0.2550(7) 0.0548(7) 0.6992(5) 0.025(2) Uani 1 1 d U . .
C19 C 0.3579(8) 0.0795(9) 0.8383(5) 0.046(3) Uani 1 1 d U . .
H19A H 0.3611 0.1468 0.8336 0.055 Uiso 1 1 calc R . .
H19B H 0.3526 0.0651 0.8914 0.055 Uiso 1 1 calc R . .
C20 C 0.4771(8) 0.0424(10) 0.8148(5) 0.042(3) Uani 1 1 d U . .
H20A H 0.4718 -0.0250 0.8173 0.051 Uiso 1 1 calc R . .
H20B H 0.5472 0.0618 0.8511 0.051 Uiso 1 1 calc R . .
S11 S 0.1717(2) 0.0854(3) 0.25014(13) 0.0417(8) Uani 1 1 d D . .
S12 S -0.1343(2) 0.0480(2) 0.31553(12) 0.0312(6) Uani 1 1 d D . .
S13 S 0.0035(2) 0.0579(2) 0.46164(12) 0.0320(6) Uani 1 1 d . . .
S14 S 0.2586(2) 0.0860(2) 0.40902(13) 0.0307(6) Uani 1 1 d . . .
S15 S 0.3823(2) 0.0818(2) 0.57797(12) 0.0295(6) Uani 1 1 d . . .
S16 S 0.12673(19) 0.0557(2) 0.63043(12) 0.0288(6) Uani 1 1 d . . .
S17 S 0.21318(18) 0.03961(18) 0.78864(11) 0.0219(5) Uani 1 1 d . . .
S18 S 0.52130(19) 0.07291(19) 0.72403(12) 0.0254(5) Uani 1 1 d . . .
C111 C 0.0309(13) 0.0583(17) 0.1975(10) 0.023(3) Uani 0.396(14) 1 d PDU A 2
H11C H 0.0370 0.0829 0.1470 0.027 Uiso 0.396(14) 1 calc PR A 2
H11D H 0.0251 -0.0090 0.1932 0.027 Uiso 0.396(14) 1 calc PR A 2
C112 C -0.0897(18) 0.0925(16) 0.2264(9) 0.025(2) Uani 0.396(14) 1 d PDU A 2
H11E H -0.1609 0.0791 0.1890 0.031 Uiso 0.396(14) 1 calc PR A 2
H11F H -0.0831 0.1597 0.2306 0.031 Uiso 0.396(14) 1 calc PR A 2
C21 C 0.1442(8) 0.3353(5) 0.1655(5) 0.0220(18) Uani 1 1 d U . .
H21A H 0.1494 0.3423 0.1115 0.026 Uiso 1 1 calc R . .
H21B H 0.1416 0.2691 0.1764 0.026 Uiso 1 1 calc R . .
C22 C 0.0201(7) 0.3781(6) 0.1869(4) 0.0202(18) Uani 1 1 d U . .
H22A H -0.0509 0.3577 0.1517 0.024 Uiso 1 1 calc R . .
H22B H 0.0268 0.4453 0.1828 0.024 Uiso 1 1 calc R . .
C23 C 0.1329(8) 0.3554(6) 0.3285(4) 0.0170(18) Uani 1 1 d U . .
C24 C 0.2487(8) 0.3686(7) 0.3049(5) 0.023(2) Uani 1 1 d U . .
C25 C 0.2888(8) 0.3543(7) 0.4457(5) 0.030(2) Uani 1 1 d U . .
C26 C 0.3400(8) 0.3555(7) 0.5179(5) 0.027(2) Uani 1 1 d U . .
C27 C 0.4948(7) 0.3634(6) 0.6364(4) 0.0184(18) Uani 1 1 d U B .
C28 C 0.3766(9) 0.3490(8) 0.6590(5) 0.029(2) Uani 1 1 d U B .
C29 C 0.4898(10) 0.3139(10) 0.7996(8) 0.028(3) Uani 0.684(15) 1 d PDU B 1
H29A H 0.4801 0.3167 0.8535 0.033 Uiso 0.684(15) 1 calc PR B 1
H29B H 0.5162 0.2509 0.7879 0.033 Uiso 0.684(15) 1 calc PR B 1
C30 C 0.5964(11) 0.3786(11) 0.7815(6) 0.029(3) Uani 0.684(15) 1 d PDU B 1
H30A H 0.6733 0.3641 0.8145 0.034 Uiso 0.684(15) 1 calc PR B 1
H30B H 0.5698 0.4415 0.7932 0.034 Uiso 0.684(15) 1 calc PR B 1
S21 S 0.28734(19) 0.38284(18) 0.21201(12) 0.0244(5) Uani 1 1 d . . .
S22 S -0.01782(19) 0.34877(18) 0.28051(13) 0.0256(5) Uani 1 1 d . . .
S23 S 0.1268(2) 0.3423(2) 0.42457(13) 0.0292(6) Uani 1 1 d . . .
S24 S 0.3794(2) 0.3706(2) 0.37009(12) 0.0287(6) Uani 1 1 d . . .
S25 S 0.5044(2) 0.3707(2) 0.54051(13) 0.0296(6) Uani 1 1 d . . .
S26 S 0.2505(2) 0.3384(2) 0.59193(13) 0.0302(6) Uani 1 1 d . . .
S27 S 0.3347(2) 0.3360(2) 0.75134(13) 0.0359(7) Uani 1 1 d D . .
S28 S 0.6412(2) 0.37658(19) 0.68734(13) 0.0286(5) Uani 1 1 d D . .
C129 C 0.4821(17) 0.362(2) 0.8001(15) 0.028(3) Uani 0.316(15) 1 d PDU B 2
H12C H 0.4925 0.4289 0.8007 0.033 Uiso 0.316(15) 1 calc PR B 2
H12D H 0.4774 0.3416 0.8520 0.033 Uiso 0.316(15) 1 calc PR B 2
C130 C 0.599(2) 0.3209(19) 0.7712(11) 0.029(3) Uani 0.316(15) 1 d PDU B 2
H13A H 0.5837 0.2552 0.7611 0.034 Uiso 0.316(15) 1 calc PR B 2
H13B H 0.6713 0.3261 0.8093 0.034 Uiso 0.316(15) 1 calc PR B 2
C31 C 0.8066(8) 0.2111(7) 0.0325(5) 0.025(2) Uani 1 1 d U . .
C32 C 0.7065(8) 0.1959(6) -0.0358(4) 0.0176(17) Uani 1 1 d U . .
O31 O 0.8659(5) 0.1401(4) 0.0564(3) 0.0258(14) Uani 1 1 d U . .
O32 O 0.6983(5) 0.1133(4) -0.0576(3) 0.0239(13) Uani 1 1 d U . .
O33 O 0.6507(6) 0.2629(5) -0.0640(4) 0.0367(17) Uani 1 1 d U . .
O34 O 0.8214(6) 0.2883(4) 0.0590(4) 0.0286(14) Uani 1 1 d U . .
C41 C 1.0312(8) -0.0531(6) 0.0500(5) 0.0234(19) Uani 1 1 d U . .
C42 C 1.0480(7) -0.0044(6) -0.0258(5) 0.0172(16) Uani 1 1 d U . .
O41 O 0.9183(6) -0.0504(4) 0.0713(3) 0.0271(13) Uani 1 1 d U . .
O42 O 0.9430(5) 0.0239(4) -0.0583(3) 0.0264(13) Uani 1 1 d U . .
O43 O 1.1557(5) 0.0038(4) -0.0489(3) 0.0281(14) Uani 1 1 d U . .
O44 O 1.1279(6) -0.0864(6) 0.0847(3) 0.0435(19) Uani 1 1 d U . .
C51 C 0.5584(8) -0.0136(6) 0.0481(5) 0.0247(19) Uani 1 1 d U . .
C52 C 0.5824(8) -0.0732(6) -0.0225(4) 0.0203(17) Uani 1 1 d U . .
O51 O 0.6556(5) 0.0240(5) 0.0760(3) 0.0291(14) Uani 1 1 d U . .
O52 O 0.6954(6) -0.0749(4) -0.0413(3) 0.0273(14) Uani 1 1 d U . .
O53 O 0.4879(6) -0.1145(5) -0.0531(3) 0.0351(15) Uani 1 1 d U . .
O54 O 0.4466(6) -0.0090(5) 0.0693(4) 0.0350(16) Uani 1 1 d U . .
C61 C 0.3237(12) 0.1952(8) 0.0232(6) 0.058(4) Uani 1 1 d U . .
H61A H 0.3697 0.2426 0.0527 0.087 Uiso 1 1 calc R . .
H61B H 0.3851 0.1587 -0.0026 0.087 Uiso 1 1 calc R . .
H61C H 0.2775 0.1557 0.0559 0.087 Uiso 1 1 calc R . .
N61 N 0.2366(9) 0.2361(7) -0.0285(5) 0.054(3) Uani 1 1 d U . .
O61 O 0.1235(7) 0.2333(6) -0.0158(5) 0.060(2) Uani 1 1 d U . .
O62 O 0.2748(6) 0.2710(5) -0.0854(3) 0.0550(17) Uani 1 1 d U . .
 
 
_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
Cr1 O32 1.984(6) . ?
Cr1 O41 1.989(6) . ?
Cr1 O42 1.992(6) . ?
Cr1 O31 1.997(6) . ?
Cr1 O52 1.999(6) . ?
Cr1 O51 2.007(6) . ?
Na1 O33 2.273(8) . ?
Na1 O54 2.303(7) 2_655 ?
Na1 O34 2.317(7) . ?
Na1 O44 2.327(7) 2_755 ?
Na1 O43 2.329(7) 2_755 ?
Na1 O53 2.366(7) 2_655 ?
C1 C2 1.500(13) . ?
C1 S1 1.778(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 S2 1.817(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.327(14) . ?
C3 S2 1.719(10) . ?
C3 S3 1.780(10) . ?
C4 S1 1.741(10) . ?
C4 S4 1.788(10) . ?
C5 C6 1.336(8) . ?
C5 S3 1.740(10) . ?
C5 S4 1.759(11) . ?
C6 S6 1.768(11) . ?
C6 S5 1.771(10) . ?
C7 C8 1.361(13) . ?
C7 S5 1.733(10) . ?
C7 S8 1.755(9) . ?
C8 S6 1.743(10) . ?
C8 S7 1.750(11) . ?
C9 C10 1.491(14) . ?
C9 S7 1.848(11) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 S8 1.798(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.514(16) . ?
C11 S11 1.821(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 S12 1.818(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.355(12) . ?
C13 S13 1.732(10) . ?
C13 S12 1.760(9) . ?
C14 S11 1.730(9) . ?
C14 S14 1.763(9) . ?
C15 C16 1.372(11) . ?
C15 S13 1.724(8) . ?
C15 S14 1.750(8) . ?
C16 S16 1.715(8) . ?
C16 S15 1.746(8) . ?
C17 C18 1.389(11) . ?
C17 S15 1.722(10) . ?
C17 S18 1.745(9) . ?
C18 S17 1.722(9) . ?
C18 S16 1.764(8) . ?
C19 C20 1.451(13) . ?
C19 S17 1.801(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 S18 1.797(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
S11 C111 1.742(13) . ?
S12 C112 1.832(13) . ?
C111 C112 1.487(17) . ?
C111 H11C 0.9900 . ?
C111 H11D 0.9900 . ?
C112 H11E 0.9900 . ?
C112 H11F 0.9900 . ?
C21 C22 1.516(11) . ?
C21 S21 1.804(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 S22 1.820(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.327(12) . ?
C23 S22 1.747(8) . ?
C23 S23 1.756(8) . ?
C24 S24 1.741(8) . ?
C24 S21 1.770(9) . ?
C25 C26 1.378(13) . ?
C25 S23 1.718(8) . ?
C25 S24 1.737(10) . ?
C26 S26 1.707(10) . ?
C26 S25 1.753(9) . ?
C27 C28 1.347(12) . ?
C27 S28 1.741(8) . ?
C27 S25 1.750(8) . ?
C28 S26 1.735(8) . ?
C28 S27 1.768(9) . ?
C29 C30 1.517(15) . ?
C29 S27 1.816(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 S28 1.801(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
S27 C129 1.761(14) . ?
S28 C130 1.807(15) . ?
C129 C130 1.49(2) . ?
C129 H12C 0.9900 . ?
C129 H12D 0.9900 . ?
C130 H13A 0.9900 . ?
C130 H13B 0.9900 . ?
C31 O34 1.234(11) . ?
C31 O31 1.271(11) . ?
C31 C32 1.578(8) . ?
C32 O33 1.234(10) . ?
C32 O32 1.274(10) . ?
C41 O44 1.251(10) . ?
C41 O41 1.268(10) . ?
C41 C42 1.570(12) . ?
C42 O43 1.235(9) . ?
C42 O42 1.277(9) . ?
O43 Na1 2.329(7) 2_745 ?
O44 Na1 2.327(7) 2_745 ?
C51 O51 1.233(10) . ?
C51 O54 1.258(9) . ?
C51 C52 1.582(12) . ?
C52 O52 1.253(10) . ?
C52 O53 1.254(10) . ?
O53 Na1 2.366(7) 2_645 ?
O54 Na1 2.303(7) 2_645 ?
C61 N61 1.394(12) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
N61 O61 1.221(11) . ?
N61 O62 1.243(10) . ?
 
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
O32 Cr1 O41 172.4(3) . . ?
O32 Cr1 O42 92.6(3) . . ?
O41 Cr1 O42 82.2(2) . . ?
O32 Cr1 O31 83.1(2) . . ?
O41 Cr1 O31 91.4(3) . . ?
O42 Cr1 O31 91.1(3) . . ?
O32 Cr1 O52 88.3(2) . . ?
O41 Cr1 O52 97.9(3) . . ?
O42 Cr1 O52 97.5(3) . . ?
O31 Cr1 O52 168.1(3) . . ?
O32 Cr1 O51 89.6(3) . . ?
O41 Cr1 O51 95.6(3) . . ?
O42 Cr1 O51 177.7(3) . . ?
O31 Cr1 O51 89.7(3) . . ?
O52 Cr1 O51 82.0(3) . . ?
O33 Na1 O54 99.6(3) . 2_655 ?
O33 Na1 O34 74.5(2) . . ?
O54 Na1 O34 169.0(3) 2_655 . ?
O33 Na1 O44 89.5(3) . 2_755 ?
O54 Na1 O44 100.1(3) 2_655 2_755 ?
O34 Na1 O44 89.2(3) . 2_755 ?
O33 Na1 O43 154.7(2) . 2_755 ?
O54 Na1 O43 101.9(3) 2_655 2_755 ?
O34 Na1 O43 86.2(2) . 2_755 ?
O44 Na1 O43 73.7(2) 2_755 2_755 ?
O33 Na1 O53 87.4(3) . 2_655 ?
O54 Na1 O53 72.5(2) 2_655 2_655 ?
O34 Na1 O53 97.7(3) . 2_655 ?
O44 Na1 O53 171.3(3) 2_755 2_655 ?
O43 Na1 O53 111.8(2) 2_755 2_655 ?
C2 C1 S1 116.4(7) . . ?
C2 C1 H1A 108.2 . . ?
S1 C1 H1A 108.2 . . ?
C2 C1 H1B 108.2 . . ?
S1 C1 H1B 108.2 . . ?
H1A C1 H1B 107.4 . . ?
C1 C2 S2 113.6(6) . . ?
C1 C2 H2A 108.8 . . ?
S2 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
S2 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 S2 129.6(8) . . ?
C4 C3 S3 117.4(7) . . ?
S2 C3 S3 113.0(6) . . ?
C3 C4 S1 129.0(8) . . ?
C3 C4 S4 117.0(7) . . ?
S1 C4 S4 114.0(6) . . ?
C6 C5 S3 122.5(6) . . ?
C6 C5 S4 122.1(5) . . ?
S3 C5 S4 115.3(6) . . ?
C5 C6 S6 122.9(5) . . ?
C5 C6 S5 122.2(6) . . ?
S6 C6 S5 114.9(6) . . ?
C8 C7 S5 118.6(7) . . ?
C8 C7 S8 128.3(8) . . ?
S5 C7 S8 113.0(5) . . ?
C7 C8 S6 117.0(8) . . ?
C7 C8 S7 127.8(8) . . ?
S6 C8 S7 115.2(6) . . ?
C10 C9 S7 113.0(8) . . ?
C10 C9 H9A 109.0 . . ?
S7 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
S7 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 S8 116.1(7) . . ?
C9 C10 H10A 108.3 . . ?
S8 C10 H10A 108.3 . . ?
C9 C10 H10B 108.3 . . ?
S8 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C4 S1 C1 99.9(5) . . ?
C3 S2 C2 101.4(5) . . ?
C5 S3 C3 95.1(5) . . ?
C5 S4 C4 94.6(5) . . ?
C7 S5 C6 94.5(5) . . ?
C8 S6 C6 95.0(5) . . ?
C8 S7 C9 102.5(5) . . ?
C7 S8 C10 102.2(5) . . ?
C12 C11 S11 117.8(10) . . ?
C12 C11 H11A 107.9 . . ?
S11 C11 H11A 107.9 . . ?
C12 C11 H11B 107.9 . . ?
S11 C11 H11B 107.9 . . ?
H11A C11 H11B 107.2 . . ?
C11 C12 S12 108.4(9) . . ?
C11 C12 H12A 110.0 . . ?
S12 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
S12 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C14 C13 S13 118.2(7) . . ?
C14 C13 S12 128.0(8) . . ?
S13 C13 S12 113.8(5) . . ?
C13 C14 S11 129.3(7) . . ?
C13 C14 S14 115.2(7) . . ?
S11 C14 S14 115.6(5) . . ?
C16 C15 S13 123.0(6) . . ?
C16 C15 S14 122.3(6) . . ?
S13 C15 S14 114.7(5) . . ?
C15 C16 S16 122.5(6) . . ?
C15 C16 S15 122.2(6) . . ?
S16 C16 S15 115.3(5) . . ?
C18 C17 S15 118.4(7) . . ?
C18 C17 S18 126.3(7) . . ?
S15 C17 S18 115.3(5) . . ?
C17 C18 S17 130.3(7) . . ?
C17 C18 S16 113.9(7) . . ?
S17 C18 S16 115.7(4) . . ?
C20 C19 S17 116.1(8) . . ?
C20 C19 H19A 108.3 . . ?
S17 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
S17 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 S18 117.2(8) . . ?
C19 C20 H20A 108.0 . . ?
S18 C20 H20A 108.0 . . ?
C19 C20 H20B 108.0 . . ?
S18 C20 H20B 108.0 . . ?
H20A C20 H20B 107.2 . . ?
C14 S11 C111 104.0(7) . . ?
C14 S11 C11 98.3(5) . . ?
C111 S11 C11 23.1(7) . . ?
C13 S12 C12 103.9(5) . . ?
C13 S12 C112 98.8(8) . . ?
C12 S12 C112 27.2(8) . . ?
C15 S13 C13 96.1(4) . . ?
C15 S14 C14 95.8(4) . . ?
C17 S15 C16 95.5(4) . . ?
C16 S16 C18 96.8(4) . . ?
C18 S17 C19 99.6(4) . . ?
C17 S18 C20 102.1(4) . . ?
C112 C111 S11 115.8(14) . . ?
C112 C111 H11C 108.3 . . ?
S11 C111 H11C 108.3 . . ?
C112 C111 H11D 108.3 . . ?
S11 C111 H11D 108.3 . . ?
H11C C111 H11D 107.4 . . ?
C111 C112 S12 117.8(13) . . ?
C111 C112 H11E 107.9 . . ?
S12 C112 H11E 107.9 . . ?
C111 C112 H11F 107.9 . . ?
S12 C112 H11F 107.9 . . ?
H11E C112 H11F 107.2 . . ?
C22 C21 S21 114.7(6) . . ?
C22 C21 H21A 108.6 . . ?
S21 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
S21 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 S22 112.8(6) . . ?
C21 C22 H22A 109.0 . . ?
S22 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
S22 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 S22 131.2(7) . . ?
C24 C23 S23 115.7(6) . . ?
S22 C23 S23 113.1(5) . . ?
C23 C24 S24 118.2(7) . . ?
C23 C24 S21 126.8(6) . . ?
S24 C24 S21 114.9(5) . . ?
C26 C25 S23 121.6(7) . . ?
C26 C25 S24 123.4(7) . . ?
S23 C25 S24 115.0(5) . . ?
C25 C26 S26 123.1(7) . . ?
C25 C26 S25 122.1(7) . . ?
S26 C26 S25 114.8(5) . . ?
C28 C27 S28 130.4(6) . . ?
C28 C27 S25 115.5(6) . . ?
S28 C27 S25 114.1(4) . . ?
C27 C28 S26 118.0(7) . . ?
C27 C28 S27 126.8(6) . . ?
S26 C28 S27 115.2(5) . . ?
C30 C29 S27 115.4(8) . . ?
C30 C29 H29A 108.4 . . ?
S27 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
S27 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 S28 116.0(10) . . ?
C29 C30 H30A 108.3 . . ?
S28 C30 H30A 108.3 . . ?
C29 C30 H30B 108.3 . . ?
S28 C30 H30B 108.3 . . ?
H30A C30 H30B 107.4 . . ?
C24 S21 C21 99.2(4) . . ?
C23 S22 C22 101.7(4) . . ?
C25 S23 C23 96.0(4) . . ?
C25 S24 C24 95.0(4) . . ?
C27 S25 C26 95.7(4) . . ?
C26 S26 C28 96.0(4) . . ?
C129 S27 C28 100.6(10) . . ?
C129 S27 C29 22.7(9) . . ?
C28 S27 C29 101.6(6) . . ?
C27 S28 C30 103.0(5) . . ?
C27 S28 C130 97.8(9) . . ?
C30 S28 C130 27.8(10) . . ?
C130 C129 S27 116.7(18) . . ?
C130 C129 H12C 108.1 . . ?
S27 C129 H12C 108.1 . . ?
C130 C129 H12D 108.1 . . ?
S27 C129 H12D 108.1 . . ?
H12C C129 H12D 107.3 . . ?
C129 C130 S28 111.7(18) . . ?
C129 C130 H13A 109.3 . . ?
S28 C130 H13A 109.3 . . ?
C129 C130 H13B 109.3 . . ?
S28 C130 H13B 109.3 . . ?
H13A C130 H13B 107.9 . . ?
O34 C31 O31 124.9(8) . . ?
O34 C31 C32 119.5(8) . . ?
O31 C31 C32 115.6(6) . . ?
O33 C32 O32 127.5(8) . . ?
O33 C32 C31 118.6(7) . . ?
O32 C32 C31 113.8(6) . . ?
C31 O31 Cr1 112.6(5) . . ?
C32 O32 Cr1 114.0(5) . . ?
C32 O33 Na1 114.6(6) . . ?
C31 O34 Na1 112.6(6) . . ?
O44 C41 O41 126.6(9) . . ?
O44 C41 C42 118.7(8) . . ?
O41 C41 C42 114.6(7) . . ?
O43 C42 O42 125.9(8) . . ?
O43 C42 C41 120.2(7) . . ?
O42 C42 C41 113.9(7) . . ?
C41 O41 Cr1 113.8(6) . . ?
C42 O42 Cr1 113.2(5) . . ?
C42 O43 Na1 110.2(5) . 2_745 ?
C41 O44 Na1 111.0(6) . 2_745 ?
O51 C51 O54 127.5(8) . . ?
O51 C51 C52 113.8(7) . . ?
O54 C51 C52 118.7(8) . . ?
O52 C52 O53 126.8(8) . . ?
O52 C52 C51 116.0(7) . . ?
O53 C52 C51 117.2(7) . . ?
C51 O51 Cr1 112.4(5) . . ?
C52 O52 Cr1 110.7(5) . . ?
C52 O53 Na1 115.0(6) . 2_645 ?
C51 O54 Na1 116.0(6) . 2_645 ?
N61 C61 H61A 109.5 . . ?
N61 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
N61 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O61 N61 O62 122.9(10) . . ?
O61 N61 C61 117.0(11) . . ?
O62 N61 C61 120.1(10) . . ?
 
_diffrn_measured_fraction_theta_max    0.995
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    1.503
_refine_diff_density_min   -0.516
_refine_diff_density_rms    0.119
