data_2009src0837

#Dr. L. Martin
#There is possible extra pseudo-symmetry observed. Due to the metal atom 
#positions it can be ignored, but it did cause problems with the displacement
#parameters for those atoms for wich the additional symmetry did hold. Thus a
#loose global thermal displacement restraint (SIMU) was used.
#There was also some disorder of the BEDT-TTF molecules and some C-S distance
#restraints were used.


 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C38 H27 Cr N Na O12 S24'
_chemical_formula_weight          1534.04
 
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'
 'Na'  'Na'   0.0362   0.0249
 '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'
 
_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                    10.4088(4)
_cell_length_b                    14.7524(8)
_cell_length_c                    18.2275(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.741(3)
_cell_angle_gamma                 90.00
_cell_volume                      2789.3(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6327
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Green
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.826
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1554
_exptl_absorpt_coefficient_mu     1.171
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9122
_exptl_absorpt_correction_T_max   0.9884
_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 17541 reflections reduced R(int) from 0.1219 to 0.0763
Ratio of minimum to maximum apparent transmission: 0.699461
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             21720
_diffrn_reflns_av_R_equivalents   0.0821
_diffrn_reflns_av_sigmaI/netI     0.1248
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          25.00
_reflns_number_total              9280
_reflns_number_gt                 5564
_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)+(0.0529P)²+33.3115P] 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    0.28(8)
_refine_ls_number_reflns          9280
_refine_ls_number_parameters      753
_refine_ls_number_restraints      592
_refine_ls_R_factor_all           0.1731
_refine_ls_R_factor_gt            0.0976
_refine_ls_wR_factor_ref          0.2397
_refine_ls_wR_factor_gt           0.1964
_refine_ls_goodness_of_fit_ref    1.090
_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
Na1 Na -0.2014(6) 0.6919(5) 0.0073(3) 0.0174(14) Uani 1 1 d . . .
Cr1 Cr 0.3046(3) 0.5601(3) 0.00424(17) 0.0350(8) Uani 1 1 d . . .
C1 C -0.002(2) 0.773(3) 0.208(2) 0.038(8) Uani 0.47(3) 1 d PDU A 1
H1A H -0.0313 0.8335 0.2232 0.046 Uiso 0.47(3) 1 calc PR A 1
H1B H 0.0056 0.7762 0.1539 0.046 Uiso 0.47(3) 1 calc PR A 1
C2 C -0.105(3) 0.706(3) 0.2211(11) 0.025(7) Uani 0.47(3) 1 d PDU A 1
H2A H -0.0744 0.6443 0.2094 0.030 Uiso 0.47(3) 1 calc PR A 1
H2B H -0.1822 0.7187 0.1870 0.030 Uiso 0.47(3) 1 calc PR A 1
C201 C 0.0120(18) 0.726(2) 0.1971(13) 0.019(6) Uani 0.53(3) 1 d PDU A 2
H20A H 0.0146 0.7535 0.1478 0.023 Uiso 0.53(3) 1 calc PR A 2
H20B H 0.0071 0.6591 0.1907 0.023 Uiso 0.53(3) 1 calc PR A 2
C202 C -0.105(3) 0.758(3) 0.2313(16) 0.042(8) Uani 0.53(3) 1 d PDU A 2
H20C H -0.1788 0.7532 0.1936 0.050 Uiso 0.53(3) 1 calc PR A 2
H20D H -0.0928 0.8236 0.2421 0.050 Uiso 0.53(3) 1 calc PR A 2
C3 C -0.0055(18) 0.7227(16) 0.3659(11) 0.044(5) Uani 1 1 d U A .
C4 C 0.1128(19) 0.7407(16) 0.3424(11) 0.044(5) Uani 1 1 d U A .
C5 C 0.1496(18) 0.7355(15) 0.4837(10) 0.041(5) Uani 1 1 d U A .
C6 C 0.2050(15) 0.7297(13) 0.5573(8) 0.027(4) Uani 1 1 d U . .
C7 C 0.3648(15) 0.7318(13) 0.6686(9) 0.024(4) Uani 1 1 d U . .
C8 C 0.2468(15) 0.7129(14) 0.6978(10) 0.033(4) Uani 1 1 d U . .
C9 C 0.3566(15) 0.7508(14) 0.8323(10) 0.033(4) Uani 1 1 d U . .
H9A H 0.3559 0.8164 0.8210 0.040 Uiso 1 1 calc R . .
H9B H 0.3539 0.7443 0.8862 0.040 Uiso 1 1 calc R . .
C10 C 0.4816(16) 0.7115(15) 0.8110(9) 0.035(4) Uani 1 1 d U . .
H10A H 0.4786 0.6447 0.8161 0.042 Uiso 1 1 calc R . .
H10B H 0.5529 0.7341 0.8455 0.042 Uiso 1 1 calc R . .
S1 S 0.1545(5) 0.7536(4) 0.2517(3) 0.0454(14) Uani 1 1 d D . .
S2 S -0.1523(4) 0.7056(5) 0.3133(3) 0.0420(14) Uani 1 1 d D . .
S3 S -0.0152(5) 0.7117(5) 0.4605(3) 0.0438(14) Uani 1 1 d . . .
S4 S 0.2399(5) 0.7491(4) 0.4101(3) 0.0391(13) Uani 1 1 d . . .
S5 S 0.3666(5) 0.7452(5) 0.5756(3) 0.0438(14) Uani 1 1 d . . .
S6 S 0.1144(4) 0.7112(4) 0.6304(3) 0.0416(14) Uani 1 1 d . . .
S7 S 0.2115(4) 0.7004(4) 0.7877(2) 0.0366(13) Uani 1 1 d . . .
S8 S 0.5148(4) 0.7395(4) 0.7184(3) 0.0400(15) Uani 1 1 d . . .
C11 C 0.597(2) 0.052(2) 0.7792(10) 0.034(6) Uani 0.68(3) 1 d PDU B 1
H11A H 0.6754 0.0424 0.8131 0.040 Uiso 0.68(3) 1 calc PR B 1
H11B H 0.5650 0.1143 0.7881 0.040 Uiso 0.68(3) 1 calc PR B 1
C12 C 0.4960(16) -0.0160(17) 0.7949(13) 0.023(5) Uani 0.68(3) 1 d PDU B 1
H12A H 0.4882 -0.0166 0.8487 0.028 Uiso 0.68(3) 1 calc PR B 1
H12B H 0.5268 -0.0766 0.7811 0.028 Uiso 0.68(3) 1 calc PR B 1
C211 C 0.604(4) -0.009(4) 0.772(2) 0.029(9) Uani 0.32(3) 1 d PDU B 2
H21A H 0.5861 -0.0741 0.7651 0.034 Uiso 0.32(3) 1 calc PR B 2
H21B H 0.6772 -0.0010 0.8096 0.034 Uiso 0.32(3) 1 calc PR B 2
C212 C 0.487(2) 0.040(3) 0.794(3) 0.029(9) Uani 0.32(3) 1 d PDU B 2
H21C H 0.4965 0.1057 0.7825 0.035 Uiso 0.32(3) 1 calc PR B 2
H21D H 0.4836 0.0346 0.8475 0.035 Uiso 0.32(3) 1 calc PR B 2
C13 C 0.3755(16) 0.0147(14) 0.6586(9) 0.030(4) Uani 1 1 d U B .
C14 C 0.4902(16) 0.0337(14) 0.6347(9) 0.033(4) Uani 1 1 d U B .
C15 C 0.3389(17) 0.0231(15) 0.5179(10) 0.038(4) Uani 1 1 d U B .
C16 C 0.2813(19) 0.0196(16) 0.4477(11) 0.046(5) Uani 1 1 d U . .
C17 C 0.2392(17) 0.0298(14) 0.3070(10) 0.034(4) Uani 1 1 d U C .
C18 C 0.1268(18) 0.0183(15) 0.3277(11) 0.038(5) Uani 1 1 d U C .
C19 C 0.027(3) 0.049(3) 0.1896(13) 0.020(6) Uani 0.48(3) 1 d PDU C 1
H19A H -0.0467 0.0396 0.1522 0.024 Uiso 0.48(3) 1 calc PR C 1
H19B H 0.0424 0.1154 0.1927 0.024 Uiso 0.48(3) 1 calc PR C 1
C20 C 0.1434(19) 0.005(3) 0.1624(18) 0.028(7) Uani 0.48(3) 1 d PDU C 1
H20E H 0.1478 0.0186 0.1094 0.033 Uiso 0.48(3) 1 calc PR C 1
H20F H 0.1387 -0.0612 0.1686 0.033 Uiso 0.48(3) 1 calc PR C 1
C219 C 0.026(2) -0.0086(19) 0.1864(10) 0.024(6) Uani 0.52(3) 1 d PDU C 2
H21E H 0.0619 -0.0705 0.1836 0.029 Uiso 0.52(3) 1 calc PR C 2
H21F H -0.0503 -0.0043 0.1503 0.029 Uiso 0.52(3) 1 calc PR C 2
C220 C 0.1248(17) 0.0592(19) 0.1677(14) 0.023(6) Uani 0.52(3) 1 d PDU C 2
H22A H 0.0913 0.1204 0.1778 0.028 Uiso 0.52(3) 1 calc PR C 2
H22B H 0.1334 0.0555 0.1141 0.028 Uiso 0.52(3) 1 calc PR C 2
S11 S 0.6395(4) 0.0438(5) 0.6849(3) 0.0459(16) Uani 1 1 d D . .
S12 S 0.3355(5) 0.0009(6) 0.7488(3) 0.066(2) Uani 1 1 d D . .
S13 S 0.2449(5) 0.0019(5) 0.5915(3) 0.0496(17) Uani 1 1 d . . .
S14 S 0.4997(4) 0.0341(5) 0.5397(3) 0.0461(16) Uani 1 1 d U . .
S15 S 0.3728(4) 0.0359(5) 0.3718(2) 0.0437(16) Uani 1 1 d . . .
S16 S 0.1198(5) 0.0055(5) 0.4238(3) 0.0439(16) Uani 1 1 d . . .
S17 S -0.0224(4) 0.0114(4) 0.2781(3) 0.0400(14) Uani 1 1 d D . .
S18 S 0.2848(4) 0.0495(4) 0.2147(2) 0.0336(12) Uani 1 1 d D . .
C21 C 1.0192(17) 0.9181(15) 0.7986(11) 0.037(5) Uani 1 1 d U . .
H21G H 1.0847 0.8723 0.7880 0.044 Uiso 1 1 calc R . .
H21H H 1.0552 0.9552 0.8406 0.044 Uiso 1 1 calc R . .
C22 C 0.9008(19) 0.8700(16) 0.8204(12) 0.049(5) Uani 1 1 d U . .
H22C H 0.8319 0.9153 0.8256 0.059 Uiso 1 1 calc R . .
H22D H 0.9207 0.8412 0.8691 0.059 Uiso 1 1 calc R . .
C23 C 0.8468(18) 0.8447(15) 0.6702(11) 0.035(5) Uani 1 1 d U . .
C24 C 0.8969(18) 0.9212(14) 0.6600(11) 0.034(4) Uani 1 1 d U . .
C25 C 0.7793(18) 0.8725(15) 0.5353(11) 0.036(4) Uani 1 1 d U . .
C26 C 0.7200(18) 0.8742(15) 0.4666(12) 0.040(5) Uani 1 1 d U . .
C27 C 0.6516(18) 0.9148(16) 0.3275(11) 0.037(5) Uani 1 1 d U . .
C28 C 0.5885(18) 0.8344(15) 0.3463(11) 0.037(5) Uani 1 1 d U . .
C29 C 0.4657(19) 0.8352(16) 0.2046(11) 0.046(5) Uani 1 1 d U . .
H29A H 0.4303 0.7975 0.1628 0.055 Uiso 1 1 calc R . .
H29B H 0.3984 0.8795 0.2156 0.055 Uiso 1 1 calc R . .
C30 C 0.5800(18) 0.8862(15) 0.1814(11) 0.039(5) Uani 1 1 d U . .
H30A H 0.5556 0.9157 0.1334 0.046 Uiso 1 1 calc R . .
H30B H 0.6497 0.8423 0.1739 0.046 Uiso 1 1 calc R . .
S21 S 0.9885(5) 0.9911(4) 0.7183(3) 0.0453(14) Uani 1 1 d . . .
S22 S 0.8414(5) 0.7844(5) 0.7553(3) 0.0524(17) Uani 1 1 d . . .
S23 S 0.7501(5) 0.7894(5) 0.5977(3) 0.0502(16) Uani 1 1 d . . .
S24 S 0.8820(6) 0.9617(5) 0.5670(3) 0.0504(17) Uani 1 1 d . . .
S25 S 0.7428(5) 0.9636(5) 0.4019(3) 0.0473(16) Uani 1 1 d . . .
S26 S 0.6121(5) 0.7903(5) 0.4330(3) 0.0521(17) Uani 1 1 d . . .
S27 S 0.4983(6) 0.7631(5) 0.2838(3) 0.0620(19) Uani 1 1 d . . .
S28 S 0.6420(5) 0.9717(4) 0.2459(3) 0.0490(16) Uani 1 1 d . . .
C31 C 0.0900(18) 0.6600(13) -0.0264(10) 0.034(4) Uani 1 1 d U . .
C32 C 0.0643(19) 0.6005(14) 0.0461(10) 0.038(4) Uani 1 1 d U . .
O31 O 0.1994(14) 0.6589(9) -0.0417(7) 0.045(4) Uani 1 1 d U . .
O32 O 0.1627(13) 0.5604(12) 0.0734(7) 0.053(4) Uani 1 1 d U . .
O33 O -0.0442(14) 0.5986(12) 0.0672(9) 0.064(4) Uani 1 1 d U . .
O34 O -0.0036(12) 0.7052(10) -0.0516(7) 0.049(3) Uani 1 1 d U . .
C41 C 0.2112(13) 0.3941(11) -0.0384(7) 0.017(3) Uani 1 1 d U . .
C42 C 0.3114(18) 0.3753(14) 0.0271(10) 0.039(4) Uani 1 1 d U . .
O41 O 0.2024(11) 0.4714(10) -0.0596(6) 0.035(3) Uani 1 1 d U . .
O42 O 0.3726(11) 0.4489(9) 0.0510(6) 0.042(3) Uani 1 1 d U . .
O43 O 0.3239(13) 0.3001(10) 0.0577(8) 0.051(4) Uani 1 1 d U . .
O44 O 0.1539(12) 0.3269(9) -0.0655(7) 0.044(3) Uani 1 1 d U . .
C51 C 0.5506(15) 0.5919(12) -0.0267(8) 0.028(4) Uani 1 1 d U . .
C52 C 0.5395(18) 0.6424(15) 0.0471(11) 0.041(4) Uani 1 1 d U . .
O51 O 0.4471(9) 0.5655(8) -0.0608(5) 0.028(3) Uani 1 1 d U . .
O52 O 0.4220(10) 0.6392(9) 0.0672(6) 0.031(3) Uani 1 1 d U . .
O53 O 0.6352(12) 0.6753(12) 0.0814(7) 0.054(4) Uani 1 1 d U . .
O54 O 0.6618(11) 0.5901(9) -0.0524(6) 0.035(3) Uani 1 1 d U . .
C61 C 0.216(2) 0.8587(19) 0.0377(16) 0.075(7) Uani 1 1 d U . .
C62 C 0.229(3) 0.900(2) -0.0306(15) 0.092(8) Uani 1 1 d U . .
H62A H 0.1741 0.8692 -0.0689 0.138 Uiso 1 1 calc R . .
H62B H 0.3194 0.8960 -0.0422 0.138 Uiso 1 1 calc R . .
H62C H 0.2040 0.9639 -0.0283 0.138 Uiso 1 1 calc R . .
N61 N 0.1972(18) 0.8259(15) 0.0926(10) 0.092(7) 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
Na1 O53 2.272(15) 1_455 ?
Na1 O54 2.282(14) 1_455 ?
Na1 O44 2.292(14) 2 ?
Na1 O43 2.309(15) 2 ?
Na1 O33 2.338(17) . ?
Na1 O34 2.406(14) . ?
Cr1 O42 1.955(13) . ?
Cr1 O31 1.968(14) . ?
Cr1 O51 1.975(10) . ?
Cr1 O52 1.984(12) . ?
Cr1 O41 1.998(13) . ?
Cr1 O32 2.020(14) . ?
C1 C2 1.500(17) . ?
C1 S1 1.780(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 S2 1.789(18) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C201 C202 1.494(17) . ?
C201 S1 1.764(17) . ?
C201 H20A 0.9900 . ?
C201 H20B 0.9900 . ?
C202 S2 1.788(18) . ?
C202 H20C 0.9900 . ?
C202 H20D 0.9900 . ?
C3 C4 1.36(3) . ?
C3 S3 1.74(2) . ?
C3 S2 1.75(2) . ?
C4 S4 1.74(2) . ?
C4 S1 1.75(2) . ?
C5 C6 1.42(2) . ?
C5 S4 1.712(19) . ?
C5 S3 1.768(19) . ?
C6 S5 1.702(17) . ?
C6 S6 1.716(16) . ?
C7 C8 1.41(2) . ?
C7 S5 1.708(16) . ?
C7 S8 1.742(17) . ?
C8 S7 1.717(19) . ?
C8 S6 1.770(17) . ?
C9 C10 1.50(2) . ?
C9 S7 1.814(16) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 S8 1.800(16) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.506(16) . ?
C11 S11 1.813(16) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 S12 1.824(16) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C211 C212 1.499(18) . ?
C211 S11 1.827(19) . ?
C211 H21A 0.9900 . ?
C211 H21B 0.9900 . ?
C212 S12 1.812(19) . ?
C212 H21C 0.9900 . ?
C212 H21D 0.9900 . ?
C13 C14 1.33(2) . ?
C13 S12 1.741(17) . ?
C13 S13 1.763(17) . ?
C14 S11 1.743(17) . ?
C14 S14 1.743(16) . ?
C15 C16 1.37(3) . ?
C15 S14 1.696(18) . ?
C15 S13 1.753(19) . ?
C16 S16 1.71(2) . ?
C16 S15 1.76(2) . ?
C17 C18 1.27(3) . ?
C17 S15 1.750(17) . ?
C17 S18 1.809(18) . ?
C18 S17 1.735(18) . ?
C18 S16 1.77(2) . ?
C19 C20 1.499(18) . ?
C19 S17 1.820(17) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 S18 1.808(17) . ?
C20 H20E 0.9900 . ?
C20 H20F 0.9900 . ?
C219 C220 1.495(17) . ?
C219 S17 1.809(16) . ?
C219 H21E 0.9900 . ?
C219 H21F 0.9900 . ?
C220 S18 1.814(15) . ?
C220 H22A 0.9900 . ?
C220 H22B 0.9900 . ?
C21 C22 1.50(3) . ?
C21 S21 1.82(2) . ?
C21 H21G 0.9900 . ?
C21 H21H 0.9900 . ?
C22 S22 1.81(2) . ?
C22 H22C 0.9900 . ?
C22 H22D 0.9900 . ?
C23 C24 1.26(3) . ?
C23 S23 1.79(2) . ?
C23 S22 1.79(2) . ?
C24 S21 1.71(2) . ?
C24 S24 1.79(2) . ?
C25 C26 1.349(17) . ?
C25 S23 1.72(2) . ?
C25 S24 1.76(2) . ?
C26 S26 1.75(2) . ?
C26 S25 1.80(2) . ?
C27 C28 1.41(3) . ?
C27 S28 1.70(2) . ?
C27 S25 1.74(2) . ?
C28 S26 1.71(2) . ?
C28 S27 1.76(2) . ?
C29 C30 1.50(3) . ?
C29 S27 1.80(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 S28 1.81(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 O31 1.19(2) . ?
C31 O34 1.24(2) . ?
C31 C32 1.63(3) . ?
C32 O33 1.22(2) . ?
C32 O32 1.25(2) . ?
C41 O41 1.205(19) . ?
C41 O44 1.240(19) . ?
C41 C42 1.544(18) . ?
C42 O43 1.24(2) . ?
C42 O42 1.31(2) . ?
O43 Na1 2.309(15) 2_545 ?
O44 Na1 2.292(14) 2_545 ?
C51 O51 1.260(18) . ?
C51 O54 1.284(18) . ?
C51 C52 1.55(3) . ?
C52 O53 1.23(2) . ?
C52 O52 1.31(2) . ?
O53 Na1 2.272(15) 1_655 ?
O54 Na1 2.282(14) 1_655 ?
C61 N61 1.14(3) . ?
C61 C62 1.40(3) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
 
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
O53 Na1 O54 75.2(5) 1_455 1_455 ?
O53 Na1 O44 87.8(6) 1_455 2 ?
O54 Na1 O44 153.5(5) 1_455 2 ?
O53 Na1 O43 88.3(6) 1_455 2 ?
O54 Na1 O43 85.1(5) 1_455 2 ?
O44 Na1 O43 74.1(5) 2 2 ?
O53 Na1 O33 100.9(6) 1_455 . ?
O54 Na1 O33 102.7(6) 1_455 . ?
O44 Na1 O33 100.3(6) 2 . ?
O43 Na1 O33 169.2(6) 2 . ?
O53 Na1 O34 169.8(5) 1_455 . ?
O54 Na1 O34 111.4(5) 1_455 . ?
O44 Na1 O34 88.6(5) 2 . ?
O43 Na1 O34 99.9(6) 2 . ?
O33 Na1 O34 70.4(5) . . ?
O42 Cr1 O31 167.4(6) . . ?
O42 Cr1 O51 91.9(5) . . ?
O31 Cr1 O51 97.7(6) . . ?
O42 Cr1 O52 93.3(5) . . ?
O31 Cr1 O52 96.0(6) . . ?
O51 Cr1 O52 82.3(5) . . ?
O42 Cr1 O41 82.0(5) . . ?
O31 Cr1 O41 89.2(5) . . ?
O51 Cr1 O41 93.8(5) . . ?
O52 Cr1 O41 173.8(5) . . ?
O42 Cr1 O32 89.3(6) . . ?
O31 Cr1 O32 81.6(6) . . ?
O51 Cr1 O32 177.0(6) . . ?
O52 Cr1 O32 94.9(5) . . ?
O41 Cr1 O32 89.0(6) . . ?
C2 C1 S1 117(2) . . ?
C2 C1 H1A 108.0 . . ?
S1 C1 H1A 108.0 . . ?
C2 C1 H1B 108.0 . . ?
S1 C1 H1B 108.0 . . ?
H1A C1 H1B 107.2 . . ?
C1 C2 S2 114(3) . . ?
C1 C2 H2A 108.7 . . ?
S2 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
S2 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C202 C201 S1 112(2) . . ?
C202 C201 H20A 109.3 . . ?
S1 C201 H20A 109.3 . . ?
C202 C201 H20B 109.3 . . ?
S1 C201 H20B 109.3 . . ?
H20A C201 H20B 108.0 . . ?
C201 C202 S2 120(2) . . ?
C201 C202 H20C 107.3 . . ?
S2 C202 H20C 107.3 . . ?
C201 C202 H20D 107.3 . . ?
S2 C202 H20D 107.3 . . ?
H20C C202 H20D 106.9 . . ?
C4 C3 S3 117.2(16) . . ?
C4 C3 S2 128.7(16) . . ?
S3 C3 S2 114.1(11) . . ?
C3 C4 S4 116.4(16) . . ?
C3 C4 S1 128.1(16) . . ?
S4 C4 S1 115.4(11) . . ?
C6 C5 S4 122.8(14) . . ?
C6 C5 S3 121.6(14) . . ?
S4 C5 S3 114.8(10) . . ?
C5 C6 S5 119.7(13) . . ?
C5 C6 S6 122.5(13) . . ?
S5 C6 S6 117.8(9) . . ?
C8 C7 S5 118.7(13) . . ?
C8 C7 S8 126.1(13) . . ?
S5 C7 S8 115.2(9) . . ?
C7 C8 S7 130.1(13) . . ?
C7 C8 S6 113.2(13) . . ?
S7 C8 S6 116.4(10) . . ?
C10 C9 S7 115.6(12) . . ?
C10 C9 H9A 108.4 . . ?
S7 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
S7 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 S8 113.0(13) . . ?
C9 C10 H10A 109.0 . . ?
S8 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
S8 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C4 S1 C201 104.2(11) . . ?
C4 S1 C1 98.9(16) . . ?
C201 S1 C1 24.2(14) . . ?
C3 S2 C202 96.2(15) . . ?
C3 S2 C2 102.7(12) . . ?
C202 S2 C2 25.7(15) . . ?
C3 S3 C5 94.8(9) . . ?
C5 S4 C4 96.6(10) . . ?
C6 S5 C7 95.0(8) . . ?
C6 S6 C8 95.2(8) . . ?
C8 S7 C9 98.5(9) . . ?
C7 S8 C10 103.9(8) . . ?
C12 C11 S11 111.1(16) . . ?
C12 C11 H11A 109.4 . . ?
S11 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
S11 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 S12 116.8(16) . . ?
C11 C12 H12A 108.1 . . ?
S12 C12 H12A 108.1 . . ?
C11 C12 H12B 108.1 . . ?
S12 C12 H12B 108.1 . . ?
H12A C12 H12B 107.3 . . ?
C212 C211 S11 105(3) . . ?
C212 C211 H21A 110.8 . . ?
S11 C211 H21A 110.8 . . ?
C212 C211 H21B 110.8 . . ?
S11 C211 H21B 110.8 . . ?
H21A C211 H21B 108.9 . . ?
C211 C212 S12 115(3) . . ?
C211 C212 H21C 108.5 . . ?
S12 C212 H21C 108.5 . . ?
C211 C212 H21D 108.5 . . ?
S12 C212 H21D 108.5 . . ?
H21C C212 H21D 107.5 . . ?
C14 C13 S12 128.6(13) . . ?
C14 C13 S13 117.1(13) . . ?
S12 C13 S13 114.3(10) . . ?
C13 C14 S11 129.0(13) . . ?
C13 C14 S14 116.8(13) . . ?
S11 C14 S14 113.6(10) . . ?
C16 C15 S14 124.8(15) . . ?
C16 C15 S13 118.7(15) . . ?
S14 C15 S13 116.1(10) . . ?
C15 C16 S16 126.0(16) . . ?
C15 C16 S15 120.4(15) . . ?
S16 C16 S15 113.6(11) . . ?
C18 C17 S15 120.4(15) . . ?
C18 C17 S18 128.1(14) . . ?
S15 C17 S18 111.4(10) . . ?
C17 C18 S17 131.3(16) . . ?
C17 C18 S16 115.0(14) . . ?
S17 C18 S16 113.7(11) . . ?
C20 C19 S17 117(2) . . ?
C20 C19 H19A 108.0 . . ?
S17 C19 H19A 108.0 . . ?
C20 C19 H19B 108.0 . . ?
S17 C19 H19B 108.0 . . ?
H19A C19 H19B 107.3 . . ?
C19 C20 S18 108(2) . . ?
C19 C20 H20E 110.0 . . ?
S18 C20 H20E 110.0 . . ?
C19 C20 H20F 110.0 . . ?
S18 C20 H20F 110.0 . . ?
H20E C20 H20F 108.4 . . ?
C220 C219 S17 110.5(17) . . ?
C220 C219 H21E 109.5 . . ?
S17 C219 H21E 109.5 . . ?
C220 C219 H21F 109.5 . . ?
S17 C219 H21F 109.5 . . ?
H21E C219 H21F 108.1 . . ?
C219 C220 S18 117.5(18) . . ?
C219 C220 H22A 107.9 . . ?
S18 C220 H22A 107.9 . . ?
C219 C220 H22B 107.9 . . ?
S18 C220 H22B 107.9 . . ?
H22A C220 H22B 107.2 . . ?
C14 S11 C11 103.3(10) . . ?
C14 S11 C211 100.6(18) . . ?
C11 S11 C211 29.1(17) . . ?
C13 S12 C212 97.0(17) . . ?
C13 S12 C12 99.8(10) . . ?
C212 S12 C12 26.7(15) . . ?
C15 S13 C13 93.7(9) . . ?
C15 S14 C14 95.5(9) . . ?
C17 S15 C16 94.1(9) . . ?
C16 S16 C18 96.8(9) . . ?
C18 S17 C219 100.7(11) . . ?
C18 S17 C19 98.0(12) . . ?
C219 S17 C19 27.3(12) . . ?
C20 S18 C17 99.7(13) . . ?
C20 S18 C220 26.3(13) . . ?
C17 S18 C220 98.7(10) . . ?
C22 C21 S21 113.4(14) . . ?
C22 C21 H21G 108.9 . . ?
S21 C21 H21G 108.9 . . ?
C22 C21 H21H 108.9 . . ?
S21 C21 H21H 108.9 . . ?
H21G C21 H21H 107.7 . . ?
C21 C22 S22 113.5(15) . . ?
C21 C22 H22C 108.9 . . ?
S22 C22 H22C 108.9 . . ?
C21 C22 H22D 108.9 . . ?
S22 C22 H22D 108.9 . . ?
H22C C22 H22D 107.7 . . ?
C24 C23 S23 120.7(16) . . ?
C24 C23 S22 127.9(17) . . ?
S23 C23 S22 110.9(11) . . ?
C23 C24 S21 131.4(17) . . ?
C23 C24 S24 115.7(16) . . ?
S21 C24 S24 112.7(12) . . ?
C26 C25 S23 122.4(12) . . ?
C26 C25 S24 120.5(12) . . ?
S23 C25 S24 116.8(12) . . ?
C25 C26 S26 122.9(12) . . ?
C25 C26 S25 123.2(12) . . ?
S26 C26 S25 113.9(12) . . ?
C28 C27 S28 129.1(16) . . ?
C28 C27 S25 113.1(15) . . ?
S28 C27 S25 117.7(13) . . ?
C27 C28 S26 120.7(16) . . ?
C27 C28 S27 125.3(15) . . ?
S26 C28 S27 113.5(13) . . ?
C30 C29 S27 114.9(15) . . ?
C30 C29 H29A 108.5 . . ?
S27 C29 H29A 108.5 . . ?
C30 C29 H29B 108.5 . . ?
S27 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 S28 114.6(14) . . ?
C29 C30 H30A 108.6 . . ?
S28 C30 H30A 108.6 . . ?
C29 C30 H30B 108.6 . . ?
S28 C30 H30B 108.6 . . ?
H30A C30 H30B 107.6 . . ?
C24 S21 C21 101.2(10) . . ?
C23 S22 C22 100.8(11) . . ?
C25 S23 C23 92.6(10) . . ?
C25 S24 C24 93.7(10) . . ?
C27 S25 C26 96.6(10) . . ?
C28 S26 C26 95.4(11) . . ?
C28 S27 C29 102.7(11) . . ?
C27 S28 C30 102.5(10) . . ?
O31 C31 O34 131.1(19) . . ?
O31 C31 C32 114.0(16) . . ?
O34 C31 C32 114.5(17) . . ?
O33 C32 O32 128(2) . . ?
O33 C32 C31 119.1(18) . . ?
O32 C32 C31 113.3(16) . . ?
C31 O31 Cr1 114.7(12) . . ?
C32 O32 Cr1 111.7(12) . . ?
C32 O33 Na1 117.9(14) . . ?
C31 O34 Na1 117.8(13) . . ?
O41 C41 O44 127.5(14) . . ?
O41 C41 C42 116.5(13) . . ?
O44 C41 C42 115.9(14) . . ?
O43 C42 O42 123.9(17) . . ?
O43 C42 C41 123.2(16) . . ?
O42 C42 C41 112.7(15) . . ?
C41 O41 Cr1 114.2(10) . . ?
C42 O42 Cr1 113.6(11) . . ?
C42 O43 Na1 110.7(12) . 2_545 ?
C41 O44 Na1 115.6(10) . 2_545 ?
O51 C51 O54 125.0(15) . . ?
O51 C51 C52 117.0(14) . . ?
O54 C51 C52 117.4(15) . . ?
O53 C52 O52 127.6(19) . . ?
O53 C52 C51 121.0(17) . . ?
O52 C52 C51 111.3(15) . . ?
C51 O51 Cr1 111.7(10) . . ?
C52 O52 Cr1 114.0(11) . . ?
C52 O53 Na1 110.8(13) . 1_655 ?
C51 O54 Na1 111.0(11) . 1_655 ?
N61 C61 C62 176(3) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    1.113
_refine_diff_density_min   -0.604
_refine_diff_density_rms    0.158
