#------------------------------------------------------------------------------
#$Date: 2024-02-12 10:29:19 +0200 (Mon, 12 Feb 2024) $
#$Revision: 289785 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/32/4513248.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4513248
loop_
_publ_author_name
'Barboiu, Mihail'
'Dumitrescu, Dan'
'Petit, Eddy'
'Legrand, Yves-Marie'
'van der Lee, Arie'
_publ_section_title
;
 Crystallization-Driven Multicomponent Encapsulation of Coulombically
 Repulsive Guests
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3525
_journal_paper_doi               10.1021/acs.cgd.5b00596
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C28 H19 Na O16.5 S4, 2(C6 H9 N2), 2(C H7 N4)'
_chemical_formula_sum            'C42 H51 N12 Na O16.5 S4'
_chemical_formula_weight         1139.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 102.545(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6234(9)
_cell_length_b                   14.1631(8)
_cell_length_c                   20.9416(11)
_cell_measurement_reflns_used    8106
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.6280
_cell_measurement_theta_min      1.9140
_cell_volume                     4812.8(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector_area_resol_mean 8.0072
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details
;
  1 omega   35.00   78.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231  179.0000 -180.0000 43

  2 omega  -46.00   60.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231  -19.0000  120.0000 106

  3 omega   -2.00   77.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231   38.0000  -30.0000 79

  4 omega  -26.00   -1.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231   19.0000 -180.0000 25

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0045699000
_diffrn_orient_matrix_UB_12      -0.0194199000
_diffrn_orient_matrix_UB_13      0.0302280000
_diffrn_orient_matrix_UB_21      -0.0365214000
_diffrn_orient_matrix_UB_22      0.0267627000
_diffrn_orient_matrix_UB_23      -0.0018733000
_diffrn_orient_matrix_UB_31      -0.0235700000
_diffrn_orient_matrix_UB_32      -0.0376444000
_diffrn_orient_matrix_UB_33      -0.0169047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.100
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24273
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.109
_diffrn_reflns_theta_min         1.749
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.96
_refine_diff_density_min         -1.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0444
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         7545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.0008942
_refine_ls_shift/su_mean         0.0000343
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 8.44 5.92 6.28 1.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1217
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0955
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                7545
_reflns_number_total             11049
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.99
_oxford_diffrn_Wilson_scale      1.16
_oxford_refine_ls_r_factor_ref   0.0820
_oxford_refine_ls_scale          1.020(3)
_oxford_reflns_number_all        11049
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            cg5b00596_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
Adding full bibliography for 4513247--4513249.cif.

2024-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C84 H102 N24 Na2 O33 S8'
_cod_original_formula_weight         2278.44
_cod_original_formula_moiety    'C56 H38 Na2 O33 S8, 4(C6 H9 N2), 4(C H7 N4)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4812.7(5)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4513248
#BEGIN Tags that were not found in dictionaries:
_cell_oxdiff_length_a            16.6243(8)
_cell_oxdiff_length_b            14.1564(8)
_cell_oxdiff_length_c            20.9485(10)
_cell_oxdiff_angle_alpha         89.981(4)
_cell_oxdiff_angle_beta          102.524(4)
_cell_oxdiff_angle_gamma         89.969(4)
_cell_oxdiff_volume              4812.7(4)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 85.52
_montpellier_reflns_redundancy_maxres 2.17
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE O   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE O   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE O   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE O   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE N   (  51,X'S) H   ( 511,X'S) H   ( 513,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE N   (  59,X'S) H   ( 593,X'S) H   ( 592,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 602,X'S) H   ( 601,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE N   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) 
RIDE N   (  69,X'S) H   ( 691,X'S) 
RIDE N   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) 
RIDE N   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE N   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE N   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE N   (  75,X'S) H   ( 751,X'S) 
RIDE N   (  76,X'S) H   ( 762,X'S) H   ( 761,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
S1 S 0.82805(6) 0.66286(7) 0.72623(4) 0.0196 1.0000 Uani .
O2 O 0.9043(2) 0.6236(3) 0.71581(16) 0.0343 1.0000 Uani .
O3 O 0.8343(2) 0.6959(2) 0.79334(13) 0.0284 1.0000 Uani .
O4 O 0.75769(19) 0.6000(2) 0.70523(14) 0.0273 1.0000 Uani .
C5 C 0.8080(2) 0.7663(3) 0.67784(16) 0.0152 1.0000 Uani .
C6 C 0.7281(2) 0.8009(3) 0.66233(17) 0.0179 1.0000 Uani .
C7 C 0.7114(2) 0.8872(3) 0.63061(16) 0.0146 1.0000 Uani .
C8 C 0.7759(2) 0.9375(3) 0.61248(16) 0.0152 1.0000 Uani .
O9 O 0.75982(16) 1.0183(2) 0.57845(12) 0.0171 1.0000 Uani .
C10 C 0.8572(2) 0.9020(3) 0.62938(16) 0.0151 1.0000 Uani .
C11 C 0.8721(2) 0.8164(3) 0.66193(17) 0.0172 1.0000 Uani .
H111 H 0.9246 0.7929 0.6726 0.0216 1.0000 Uiso R
C12 C 0.9262(2) 0.9553(3) 0.60757(17) 0.0186 1.0000 Uani .
C13 C 0.9356(2) 0.9187(3) 0.54168(17) 0.0166 1.0000 Uani .
C14 C 0.8886(2) 0.9560(3) 0.48292(17) 0.0148 1.0000 Uani .
O15 O 0.83831(17) 1.0313(2) 0.48334(12) 0.0211 1.0000 Uani .
C16 C 0.8943(2) 0.9169(3) 0.42276(18) 0.0168 1.0000 Uani .
C17 C 0.9482(2) 0.8423(3) 0.42213(18) 0.0184 1.0000 Uani .
C18 C 0.9952(2) 0.8062(3) 0.48050(19) 0.0191 1.0000 Uani .
C19 C 0.9891(2) 0.8447(3) 0.53945(19) 0.0194 1.0000 Uani .
H191 H 1.0201 0.8204 0.5784 0.0229 1.0000 Uiso R
S20 S 1.06164(6) 0.70885(8) 0.48107(5) 0.0232 1.0000 Uani .
O21 O 1.12292(19) 0.7149(2) 0.54148(15) 0.0287 1.0000 Uani .
Na22 Na 1.21930(11) 0.82823(13) 0.58620(8) 0.0272 1.0000 Uani .
O23 O 1.1988(2) 0.8141(3) 0.69394(16) 0.0382 1.0000 Uani .
S24 S 1.15850(6) 0.82857(7) 0.74783(5) 0.0210 1.0000 Uani .
O25 O 1.1991(2) 0.9013(2) 0.79342(16) 0.0352 1.0000 Uani .
O26 O 1.07119(19) 0.8473(2) 0.72854(15) 0.0326 1.0000 Uani .
C27 C 0.6714(2) 0.7770(3) 0.29380(16) 0.0160 1.0000 Uani .
C28 C 0.6039(2) 0.8152(3) 0.31365(17) 0.0166 1.0000 Uani .
C29 C 0.6112(2) 0.9009(3) 0.34745(16) 0.0151 1.0000 Uani .
C30 C 0.6867(2) 0.9482(3) 0.35862(16) 0.0150 1.0000 Uani .
O31 O 1.30687(16) 0.9623(2) 0.61558(12) 0.0179 1.0000 Uani .
C32 C 0.7569(2) 0.9075(3) 0.34218(16) 0.0149 1.0000 Uani .
C33 C 0.7470(2) 0.8215(3) 0.30872(17) 0.0171 1.0000 Uani .
H331 H 0.7918 0.7937 0.2966 0.0204 1.0000 Uiso R
C34 C 0.8407(2) 0.9535(3) 0.35897(17) 0.0179 1.0000 Uani .
H341 H 0.8572 0.9985 0.3340 0.0231 1.0000 Uiso R
C35 C 0.5366(2) 0.9399(3) 0.36917(16) 0.0159 1.0000 Uani .
C36 C 0.5256(2) 0.8993(3) 0.43389(16) 0.0147 1.0000 Uani .
C37 C 0.5774(2) 0.9289(3) 0.49239(17) 0.0153 1.0000 Uani .
O38 O 0.63513(16) 0.9947(2) 0.48791(12) 0.0189 1.0000 Uani .
C39 C 0.5696(2) 0.8924(3) 0.55341(16) 0.0140 1.0000 Uani .
C40 C 0.6248(2) 0.9264(3) 0.61647(16) 0.0166 1.0000 Uani .
H401 H 0.5988 0.9064 0.6518 0.0201 1.0000 Uiso R
H402 H 0.6279 0.9947 0.6155 0.0202 1.0000 Uiso R
C41 C 0.5066(2) 0.8285(3) 0.55376(18) 0.0202 1.0000 Uani .
C42 C 0.4533(2) 0.7999(3) 0.49607(18) 0.0171 1.0000 Uani .
C43 C 0.4637(2) 0.8352(3) 0.43646(17) 0.0170 1.0000 Uani .
H431 H 0.4284 0.8152 0.3981 0.0199 1.0000 Uiso R
S44 S 0.36761(6) 0.72896(8) 0.49973(5) 0.0252 1.0000 Uani .
O45 O 0.3104(3) 0.7889(4) 0.5229(3) 0.0708 1.0000 Uani .
O46 O 0.3322(2) 0.6993(3) 0.43434(17) 0.0481 1.0000 Uani .
O47 O 0.3961(3) 0.6530(3) 0.5441(2) 0.0612 1.0000 Uani .
H411 H 0.4991 0.8038 0.5935 0.0241 1.0000 Uiso R
H351 H 0.4884 0.9251 0.3357 0.0189 1.0000 Uiso R
H352 H 0.5407 1.0081 0.3732 0.0188 1.0000 Uiso R
H281 H 0.5538 0.7839 0.3033 0.0204 1.0000 Uiso R
O48 O 1.0953(2) 0.7172(3) 0.42337(16) 0.0372 1.0000 Uani .
O49 O 1.0105(2) 0.6247(3) 0.48117(16) 0.0350 1.0000 Uani .
H171 H 0.9531 0.8162 0.3830 0.0222 1.0000 Uiso R
H121 H 0.9769 0.9452 0.6387 0.0217 1.0000 Uiso R
H122 H 0.9135 1.0220 0.6049 0.0223 1.0000 Uiso R
H61 H 0.6855 0.7663 0.6732 0.0207 1.0000 Uiso R
O50 O 1.2825(10) 0.6640(14) 0.6298(7) 0.1476 0.5000 Uani .
H501 H 1.3157 0.6607 0.6042 0.1609 0.5000 Uiso R
H502 H 1.3300 0.6621 0.6551 0.1609 0.5000 Uiso R
N51 N 0.7016(2) 0.6817(3) 0.85795(18) 0.0287 1.0000 Uani .
C52 C 0.6354(3) 0.6565(3) 0.7981(2) 0.0312 1.0000 Uani .
C53 C 0.5732(3) 0.7336(3) 0.77637(19) 0.0281 1.0000 Uani .
N54 N 0.5990(2) 0.8230(3) 0.78639(17) 0.0270 1.0000 Uani .
C55 C 0.5415(3) 0.8907(4) 0.7673(2) 0.0369 1.0000 Uani .
C56 C 0.4612(3) 0.8728(5) 0.7385(2) 0.0436 1.0000 Uani .
C57 C 0.4360(3) 0.7806(5) 0.7270(2) 0.0496 1.0000 Uani .
C58 C 0.4931(3) 0.7094(4) 0.7462(2) 0.0414 1.0000 Uani .
H581 H 0.4789 0.6465 0.7391 0.0490 1.0000 Uiso R
H571 H 0.3817 0.7668 0.7072 0.0598 1.0000 Uiso R
H561 H 0.4234 0.9223 0.7270 0.0518 1.0000 Uiso R
H551 H 0.5581 0.9533 0.7748 0.0442 1.0000 Uiso R
H521 H 0.6611 0.6400 0.7629 0.0379 1.0000 Uiso R
H522 H 0.6056 0.6024 0.8088 0.0383 1.0000 Uiso R
H511 H 0.7188 0.6306 0.8810 0.0429 1.0000 Uiso R
H513 H 0.6822 0.7230 0.8827 0.0428 1.0000 Uiso R
H512 H 0.7433 0.7066 0.8454 0.0430 1.0000 Uiso R
N59 N 0.7740(3) 0.4436(3) 0.62736(19) 0.0325 1.0000 Uani .
C60 C 0.8147(3) 0.4868(4) 0.5794(3) 0.0442 1.0000 Uani .
C61 C 0.7698(3) 0.5712(3) 0.5465(2) 0.0289 1.0000 Uani .
N62 N 0.6884(3) 0.5710(3) 0.5386(2) 0.0384 1.0000 Uani .
C63 C 0.6474(4) 0.6421(5) 0.5060(3) 0.0535 1.0000 Uani .
C64 C 0.6850(5) 0.7153(5) 0.4812(3) 0.0599 1.0000 Uani .
C65 C 0.7689(5) 0.7176(5) 0.4919(3) 0.0559 1.0000 Uani .
C66 C 0.8131(4) 0.6443(4) 0.5254(3) 0.0456 1.0000 Uani .
H661 H 0.8706 0.6435 0.5341 0.0541 1.0000 Uiso R
H651 H 0.7955 0.7680 0.4763 0.0669 1.0000 Uiso R
H641 H 0.6540 0.7631 0.4574 0.0711 1.0000 Uiso R
H631 H 0.5909 0.6415 0.4996 0.0650 1.0000 Uiso R
H602 H 0.8178 0.4407 0.5460 0.0530 1.0000 Uiso R
H601 H 0.8701 0.5061 0.6012 0.0531 1.0000 Uiso R
H593 H 0.7283 0.4164 0.6061 0.0486 1.0000 Uiso R
H592 H 0.8067 0.4000 0.6508 0.0487 1.0000 Uiso R
H591 H 0.7608 0.4874 0.6536 0.0487 1.0000 Uiso R
N67 N 0.8285(3) 0.4693(4) 0.3069(2) 0.0439 1.0000 Uani .
C68 C 0.8800(3) 0.5060(4) 0.3565(2) 0.0301 1.0000 Uani .
N69 N 0.9515(2) 0.4625(3) 0.38009(18) 0.0356 1.0000 Uani .
N70 N 0.9600(3) 0.3731(3) 0.3541(2) 0.0441 1.0000 Uani .
H701 H 1.0045 0.3613 0.3410 0.0529 1.0000 Uiso R
H702 H 0.9540 0.3238 0.3766 0.0535 1.0000 Uiso R
H691 H 0.9802 0.4762 0.4188 0.0431 1.0000 Uiso R
N71 N 0.8647(3) 0.5874(4) 0.3826(2) 0.0500 1.0000 Uani .
H711 H 0.8995 0.6091 0.4161 0.0599 1.0000 Uiso R
H712 H 0.8157 0.6089 0.3746 0.0599 1.0000 Uiso R
H672 H 0.8381 0.4139 0.2926 0.0532 1.0000 Uiso R
H671 H 0.7827 0.4976 0.2913 0.0531 1.0000 Uiso R
N72 N 0.5309(3) 0.5325(4) 0.6025(3) 0.0610 1.0000 Uani .
C73 C 0.4922(4) 0.4883(4) 0.6426(3) 0.0417 1.0000 Uani .
N74 N 0.4137(3) 0.5049(4) 0.6403(3) 0.0517 1.0000 Uani .
H742 H 0.3883 0.4748 0.6655 0.0619 1.0000 Uiso R
H741 H 0.3880 0.5478 0.6145 0.0619 1.0000 Uiso R
N75 N 0.5325(3) 0.4260(4) 0.6857(2) 0.0460 1.0000 Uani .
N76 N 0.6164(3) 0.4103(3) 0.6887(2) 0.0437 1.0000 Uani .
H762 H 0.6513 0.4200 0.7254 0.0522 1.0000 Uiso R
H761 H 0.6316 0.3527 0.6820 0.0530 1.0000 Uiso R
H751 H 0.5093 0.4015 0.7144 0.0548 1.0000 Uiso R
H721 H 0.5087 0.5809 0.5804 0.0730 1.0000 Uiso R
H722 H 0.5829 0.5243 0.6063 0.0730 1.0000 Uiso R
H151 H 0.8111 1.0198 0.5171 0.0500 1.0000 Uiso R
H381 H 0.6696 1.0020 0.5236 0.0500 1.0000 Uiso R
H311 H 1.3244 0.9798 0.5800 0.0500 1.0000 Uiso R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_montpellier_diffrn_reflns_class_number
_montpellier_diffrn_reflns_class_d_res_high
_montpellier_diffrn_reflns_class_d_res_low
_montpellier_diffrn_reflns_class_redundancy
_montpellier_diffrn_reflns_class_av_i/ui
_diffrn_reflns_class_av_R_eq
_montpellier_diffrn_reflns_class_completeness_shell
_montpellier_diffrn_reflns_class_cumul_completeness
0 100.0 1.68 3.4 30.44 0.079 99.7 99.65
1 1.68 1.33 2.8 12.41 0.107 100.0 99.83
2 1.33 1.16 2.6 9.42 0.112 99.8 99.83
3 1.16 1.05 2.3 7.26 0.127 99.6 99.76
4 1.05 0.97 2.1 5.17 0.137 99.4 99.69
5 0.97 0.91 2.0 4.10 0.164 99.5 99.65
6 0.91 0.87 1.9 3.23 0.166 98.8 99.53
7 0.87 0.83 1.7 2.85 0.174 98.6 99.42
8 0.83 0.80 1.6 2.54 0.187 97.8 99.23
9 0.80 0.73 1.3 2.04 0.209 38.1 85.52
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 . S1 O3 . 112.8(2) yes
O2 . S1 O4 . 113.1(2) yes
O3 . S1 O4 . 111.68(18) yes
O2 . S1 C5 . 107.13(18) yes
O3 . S1 C5 . 104.52(18) yes
O4 . S1 C5 . 107.04(18) yes
S1 . C5 C6 . 118.6(3) yes
S1 . C5 C11 . 120.3(3) yes
C6 . C5 C11 . 120.8(4) yes
C5 . C6 C7 . 120.3(4) yes
C5 . C6 H61 . 119.9 no
C7 . C6 H61 . 119.8 no
C6 . C7 C8 . 119.3(3) yes
C6 . C7 C40 . 120.0(3) yes
C8 . C7 C40 . 120.7(3) yes
C7 . C8 O9 . 120.0(3) yes
C7 . C8 C10 . 119.8(3) yes
O9 . C8 C10 . 120.3(3) yes
C8 . C10 C11 . 119.5(3) yes
C8 . C10 C12 . 119.4(3) yes
C11 . C10 C12 . 120.9(3) yes
C10 . C11 C5 . 120.2(3) yes
C10 . C11 H111 . 119.8 no
C5 . C11 H111 . 119.9 no
C10 . C12 C13 . 109.7(3) yes
C10 . C12 H121 . 109.3 no
C13 . C12 H121 . 108.6 no
C10 . C12 H122 . 109.4 no
C13 . C12 H122 . 110.2 no
H121 . C12 H122 . 109.4 no
C12 . C13 C14 . 121.3(3) yes
C12 . C13 C19 . 119.0(3) yes
C14 . C13 C19 . 119.6(3) yes
C13 . C14 O15 . 121.0(3) yes
C13 . C14 C16 . 120.3(3) yes
O15 . C14 C16 . 118.7(3) yes
C14 . O15 Na22 2_776 140.5(2) yes
C14 . O15 H151 . 105.6 no
Na22 2_776 O15 H151 . 112.9 no
C14 . C16 C17 . 118.8(3) yes
C14 . C16 C34 . 120.8(3) yes
C17 . C16 C34 . 120.4(3) yes
C16 . C17 C18 . 120.7(3) yes
C16 . C17 H171 . 119.8 no
C18 . C17 H171 . 119.5 no
C17 . C18 C19 . 120.3(4) yes
C17 . C18 S20 . 121.5(3) yes
C19 . C18 S20 . 118.2(3) yes
C13 . C19 C18 . 120.3(4) yes
C13 . C19 H191 . 119.3 no
C18 . C19 H191 . 120.4 no
C18 . S20 O21 . 106.34(19) yes
C18 . S20 O48 . 106.66(19) yes
O21 . S20 O48 . 113.6(2) yes
C18 . S20 O49 . 105.80(19) yes
O21 . S20 O49 . 110.3(2) yes
O48 . S20 O49 . 113.5(2) yes
S20 . O21 Na22 . 133.6(2) yes
O21 . Na22 O45 1_655 94.80(15) yes
O21 . Na22 O15 2_776 99.80(12) yes
O45 1_655 Na22 O15 2_776 94.21(17) yes
O21 . Na22 O23 . 95.55(14) yes
O45 1_655 Na22 O23 . 141.6(2) yes
O15 2_776 Na22 O23 . 120.10(13) yes
O21 . Na22 O31 . 169.51(13) yes
O45 1_655 Na22 O31 . 84.25(14) yes
O15 2_776 Na22 O31 . 69.90(10) yes
O23 . Na22 O31 . 91.59(13) yes
O21 . Na22 O50 . 73.6(5) yes
O45 1_655 Na22 O50 . 73.8(3) yes
O15 2_776 Na22 O50 . 165.4(4) yes
O23 . Na22 O50 . 74.0(3) yes
O31 . Na22 O50 . 116.0(5) yes
Na22 . O23 S24 . 157.0(2) yes
C27 3_565 S24 O23 . 106.48(19) yes
C27 3_565 S24 O25 . 104.82(18) yes
O23 . S24 O25 . 112.5(2) yes
C27 3_565 S24 O26 . 107.65(18) yes
O23 . S24 O26 . 114.5(2) yes
O25 . S24 O26 . 110.2(2) yes
S24 3_464 C27 C28 . 118.9(3) yes
S24 3_464 C27 C33 . 120.4(3) yes
C28 . C27 C33 . 120.7(4) yes
C27 . C28 C29 . 120.2(4) yes
C27 . C28 H281 . 119.2 no
C29 . C28 H281 . 120.6 no
C28 . C29 C30 . 118.5(3) yes
C28 . C29 C35 . 118.8(3) yes
C30 . C29 C35 . 122.7(3) yes
C29 . C30 O31 2_776 119.9(3) yes
C29 . C30 C32 . 121.6(3) yes
O31 2_776 C30 C32 . 118.5(3) yes
Na22 . O31 C30 2_776 145.6(2) yes
Na22 . O31 H311 . 107.2 no
C30 2_776 O31 H311 . 93.5 no
C30 . C32 C33 . 117.8(3) yes
C30 . C32 C34 . 122.5(3) yes
C33 . C32 C34 . 119.8(3) yes
C32 . C33 C27 . 120.9(3) yes
C32 . C33 H331 . 119.7 no
C27 . C33 H331 . 119.4 no
C16 . C34 C32 . 113.0(3) yes
C16 . C34 H341 . 123.5 no
C32 . C34 H341 . 123.5 no
C29 . C35 C36 . 113.2(3) yes
C29 . C35 H351 . 107.9 no
C36 . C35 H351 . 108.9 no
C29 . C35 H352 . 109.9 no
C36 . C35 H352 . 108.6 no
H351 . C35 H352 . 108.1 no
C35 . C36 C37 . 119.8(3) yes
C35 . C36 C43 . 121.2(3) yes
C37 . C36 C43 . 119.0(3) yes
C36 . C37 O38 . 117.1(3) yes
C36 . C37 C39 . 121.5(3) yes
O38 . C37 C39 . 121.4(3) yes
C37 . O38 H381 . 112.2 no
C37 . C39 C40 . 121.1(3) yes
C37 . C39 C41 . 117.6(3) yes
C40 . C39 C41 . 121.3(3) yes
C39 . C40 C7 . 115.2(3) yes
C39 . C40 H401 . 106.5 no
C7 . C40 H401 . 107.8 no
C39 . C40 H402 . 108.9 no
C7 . C40 H402 . 108.7 no
H401 . C40 H402 . 109.8 no
C39 . C41 C42 . 121.6(3) yes
C39 . C41 H411 . 119.7 no
C42 . C41 H411 . 118.7 no
C41 . C42 C43 . 119.6(4) yes
C41 . C42 S44 . 119.8(3) yes
C43 . C42 S44 . 120.3(3) yes
C42 . C43 C36 . 120.7(3) yes
C42 . C43 H431 . 119.2 no
C36 . C43 H431 . 120.1 no
C42 . S44 O45 . 106.2(2) yes
C42 . S44 O46 . 107.2(2) yes
O45 . S44 O46 . 109.4(3) yes
C42 . S44 O47 . 107.5(2) yes
O45 . S44 O47 . 112.0(3) yes
O46 . S44 O47 . 114.2(3) yes
Na22 1_455 O45 S44 . 155.6(4) yes
Na22 . O50 H501 . 95.5 no
Na22 . O50 H502 . 119.4 no
H501 . O50 H502 . 75.5 no
C52 . N51 H511 . 110.4 no
C52 . N51 H513 . 110.2 no
H511 . N51 H513 . 109.6 no
C52 . N51 H512 . 109.2 no
H511 . N51 H512 . 108.4 no
H513 . N51 H512 . 109.0 no
N51 . C52 C53 . 114.0(4) yes
N51 . C52 H521 . 109.1 no
C53 . C52 H521 . 109.6 no
N51 . C52 H522 . 108.2 no
C53 . C52 H522 . 107.0 no
H521 . C52 H522 . 108.8 no
C52 . C53 N54 . 117.6(4) yes
C52 . C53 C58 . 119.2(5) yes
N54 . C53 C58 . 123.2(5) yes
C53 . N54 C55 . 116.3(4) yes
N54 . C55 C56 . 124.1(5) yes
N54 . C55 H551 . 117.5 no
C56 . C55 H551 . 118.4 no
C55 . C56 C57 . 119.0(5) yes
C55 . C56 H561 . 120.8 no
C57 . C56 H561 . 120.2 no
C56 . C57 C58 . 118.5(5) yes
C56 . C57 H571 . 120.4 no
C58 . C57 H571 . 121.1 no
C53 . C58 C57 . 118.9(6) yes
C53 . C58 H581 . 119.8 no
C57 . C58 H581 . 121.3 no
C60 . N59 H593 . 108.2 no
C60 . N59 H592 . 110.4 no
H593 . N59 H592 . 109.3 no
C60 . N59 H591 . 110.2 no
H593 . N59 H591 . 108.5 no
H592 . N59 H591 . 110.2 no
N59 . C60 C61 . 113.0(4) yes
N59 . C60 H602 . 108.6 no
C61 . C60 H602 . 107.8 no
N59 . C60 H601 . 109.1 no
C61 . C60 H601 . 108.6 no
H602 . C60 H601 . 109.6 no
C60 . C61 N62 . 116.7(4) yes
C60 . C61 C66 . 120.1(5) yes
N62 . C61 C66 . 123.2(5) yes
C61 . N62 C63 . 117.4(5) yes
N62 . C63 C64 . 123.2(6) yes
N62 . C63 H631 . 117.7 no
C64 . C63 H631 . 119.2 no
C63 . C64 C65 . 119.3(5) yes
C63 . C64 H641 . 120.6 no
C65 . C64 H641 . 120.0 no
C64 . C65 C66 . 118.8(6) yes
C64 . C65 H651 . 120.3 no
C66 . C65 H651 . 120.9 no
C61 . C66 C65 . 118.0(6) yes
C61 . C66 H661 . 120.7 no
C65 . C66 H661 . 121.3 no
C68 . N67 H672 . 119.9 no
C68 . N67 H671 . 119.5 no
H672 . N67 H671 . 120.3 no
N67 . C68 N69 . 119.3(5) yes
N67 . C68 N71 . 121.6(4) yes
N69 . C68 N71 . 119.0(4) yes
C68 . N69 N70 . 115.6(4) yes
C68 . N69 H691 . 120.4 no
N70 . N69 H691 . 119.0 no
N69 . N70 H701 . 117.9 no
N69 . N70 H702 . 119.2 no
H701 . N70 H702 . 103.0 no
C68 . N71 H711 . 119.3 no
C68 . N71 H712 . 119.4 no
H711 . N71 H712 . 118.7 no
C73 . N72 H721 . 120.4 no
C73 . N72 H722 . 119.7 no
H721 . N72 H722 . 117.5 no
N72 . C73 N74 . 120.5(5) yes
N72 . C73 N75 . 120.0(5) yes
N74 . C73 N75 . 119.5(5) yes
C73 . N74 H742 . 120.4 no
C73 . N74 H741 . 120.2 no
H742 . N74 H741 . 119.4 no
C73 . N75 N76 . 119.0(4) yes
C73 . N75 H751 . 120.4 no
N76 . N75 H751 . 120.1 no
N75 . N76 H762 . 118.7 no
N75 . N76 H761 . 117.5 no
H762 . N76 H761 . 97.4 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O2 . 1.444(3) yes
S1 O3 . 1.463(3) yes
S1 O4 . 1.460(3) yes
S1 C5 . 1.771(4) yes
C5 C6 . 1.387(5) yes
C5 C11 . 1.380(5) yes
C6 C7 . 1.390(5) yes
C6 H61 . 0.930 no
C7 C8 . 1.406(5) yes
C7 C40 . 1.510(5) yes
C8 O9 . 1.344(4) yes
C8 C10 . 1.413(5) yes
C10 C11 . 1.387(5) yes
C10 C12 . 1.523(5) yes
C11 H111 . 0.916 no
C12 C13 . 1.514(5) yes
C12 H121 . 0.959 no
C12 H122 . 0.967 no
C13 C14 . 1.409(5) yes
C13 C19 . 1.382(6) yes
C14 O15 . 1.356(5) yes
C14 C16 . 1.399(5) yes
O15 Na22 2_776 2.528(3) yes
O15 H151 . 0.932 no
C16 C17 . 1.387(6) yes
C16 C34 . 1.527(5) yes
C17 C18 . 1.397(5) yes
C17 H171 . 0.919 no
C18 C19 . 1.373(6) yes
C18 S20 . 1.765(4) yes
C19 H191 . 0.931 no
S20 O21 . 1.444(3) yes
S20 O48 . 1.442(3) yes
S20 O49 . 1.464(4) yes
O21 Na22 . 2.317(4) yes
Na22 O45 1_655 2.286(4) yes
Na22 O23 . 2.363(3) yes
Na22 O31 . 2.391(3) yes
Na22 O50 . 2.632(17) yes
O23 S24 . 1.446(3) yes
S24 C27 3_565 1.766(4) yes
S24 O25 . 1.465(3) yes
S24 O26 . 1.444(3) yes
C27 C28 . 1.388(5) yes
C27 C33 . 1.381(5) yes
C28 C29 . 1.397(5) yes
C28 H281 . 0.927 no
C29 C30 . 1.397(5) yes
C29 C35 . 1.515(5) yes
C30 O31 2_776 1.372(5) yes
C30 C32 . 1.410(5) yes
O31 H311 . 0.892 no
C32 C33 . 1.396(5) yes
C32 C34 . 1.508(5) yes
C33 H331 . 0.925 no
C34 H341 . 0.904 no
C35 C36 . 1.520(5) yes
C35 H351 . 0.965 no
C35 H352 . 0.971 no
C36 C37 . 1.400(5) yes
C36 C43 . 1.381(5) yes
C37 O38 . 1.356(5) yes
C37 C39 . 1.410(5) yes
O38 H381 . 0.843 no
C39 C40 . 1.514(5) yes
C39 C41 . 1.385(6) yes
C40 H401 . 0.978 no
C40 H402 . 0.968 no
C41 C42 . 1.394(5) yes
C41 H411 . 0.936 no
C42 C43 . 1.390(5) yes
C42 S44 . 1.758(4) yes
C43 H431 . 0.930 no
S44 O45 . 1.437(4) yes
S44 O46 . 1.431(4) yes
S44 O47 . 1.433(4) yes
O50 H501 . 0.850 no
O50 H502 . 0.850 no
N51 C52 . 1.520(6) yes
N51 H511 . 0.882 no
N51 H513 . 0.887 no
N51 H512 . 0.869 no
C52 C53 . 1.504(7) yes
C52 H521 . 0.959 no
C52 H522 . 0.964 no
C53 N54 . 1.339(6) yes
C53 C58 . 1.386(7) yes
N54 C55 . 1.351(6) yes
C55 C56 . 1.364(8) yes
C55 H551 . 0.931 no
C56 C57 . 1.377(9) yes
C56 H561 . 0.938 no
C57 C58 . 1.383(9) yes
C57 H571 . 0.928 no
C58 H581 . 0.927 no
N59 C60 . 1.463(7) yes
N59 H593 . 0.883 no
N59 H592 . 0.895 no
N59 H591 . 0.889 no
C60 C61 . 1.496(7) yes
C60 H602 . 0.966 no
C60 H601 . 0.973 no
C61 N62 . 1.327(6) yes
C61 C66 . 1.387(7) yes
N62 C63 . 1.319(7) yes
C63 C64 . 1.370(10) yes
C63 H631 . 0.920 no
C64 C65 . 1.363(11) yes
C64 H641 . 0.928 no
C65 C66 . 1.373(9) yes
C65 H651 . 0.935 no
C66 H661 . 0.934 no
N67 C68 . 1.303(6) yes
N67 H672 . 0.867 no
N67 H671 . 0.860 no
C68 N69 . 1.335(6) yes
C68 N71 . 1.324(7) yes
N69 N70 . 1.397(7) yes
N69 H691 . 0.868 no
N70 H701 . 0.860 no
N70 H702 . 0.860 no
N71 H711 . 0.863 no
N71 H712 . 0.850 no
N72 C73 . 1.322(7) yes
N72 H721 . 0.864 no
N72 H722 . 0.860 no
C73 N74 . 1.315(7) yes
C73 N75 . 1.335(7) yes
N74 H742 . 0.858 no
N74 H741 . 0.862 no
N75 N76 . 1.399(7) yes
N75 H751 . 0.855 no
N76 H762 . 0.868 no
N76 H761 . 0.874 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C11 H111 O26 . 139.32(12) 0.916 2.581 3.329(6) yes
C43 H431 O3 3_464 166.04(12) 0.930 2.407 3.317(6) yes
C12 H121 O26 . 151.99(11) 0.959 2.576 3.452(6) yes
O50 H501 O47 1_655 179.3(5) 0.850 2.028 2.878(6) yes
C57 H571 O50 1_455 148.1(4) 0.928 2.512 3.336(6) yes
C55 H551 O2 4_656 174.75(13) 0.931 2.488 3.417(6) yes
C52 H521 O4 . 162.01(14) 0.959 2.281 3.206(6) yes
N51 H511 O9 4_646 171.61(15) 0.882 1.801 2.678(6) yes
N51 H513 O48 3_465 155.32(15) 0.887 2.017 2.847(6) yes
N51 H512 O3 . 149.31(14) 0.869 2.052 2.834(6) yes
N59 H593 O46 2_666 149.97(17) 0.883 2.010 2.809(6) yes
N59 H592 N54 4_646 167.26(15) 0.895 2.117 2.996(6) yes
N59 H591 O4 . 164.42(16) 0.889 1.933 2.799(6) yes
N70 H701 O2 2_766 157.52(15) 0.860 2.131 2.944(6) yes
N70 H702 O21 2_766 135.68(13) 0.860 2.416 3.090(6) yes
N69 H691 O49 . 133.81(12) 0.868 2.470 3.134(6) yes
N69 H691 O49 2_766 124.85(13) 0.868 2.514 3.093(6) yes
N71 H711 O49 . 157.79(16) 0.863 2.053 2.870(6) yes
N71 H712 O25 3_464 138.18(14) 0.850 2.289 2.976(6) yes
N67 H671 O25 3_464 152.38(15) 0.860 2.003 2.793(6) yes
N74 H742 O25 4_646 165.51(16) 0.858 2.116 2.955(6) yes
N74 H741 O47 . 146.36(18) 0.862 2.122 2.879(6) yes
N74 H741 O50 1_455 131.1(3) 0.862 2.476 3.111(6) yes
N76 H761 O3 4_646 157.18(13) 0.874 2.323 3.147(6) yes
N75 H751 O26 4_646 168.11(16) 0.855 2.121 2.964(6) yes
N72 H721 O47 . 144.54(16) 0.864 2.123 2.871(6) yes
N72 H722 N62 . 135.03(15) 0.860 2.569 3.235(6) yes
O15 H151 C8 . 158.02(11) 0.932 2.491 3.373(6) yes
O15 H151 O9 . 170.63(13) 0.932 1.690 2.614(6) yes
O38 H381 C8 . 150.14(11) 0.843 2.449 3.207(6) yes
O38 H381 O9 . 161.38(12) 0.843 1.696 2.509(6) yes
O31 H311 O38 2_776 174.75(13) 0.892 1.738 2.627(6) yes
