#------------------------------------------------------------------------------
#$Date: 2017-05-27 04:43:47 +0300 (Sat, 27 May 2017) $
#$Revision: 197009 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/83/7228320.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_7228320
loop_
_publ_author_name
'Pinalli, Roberta'
'Brancatelli, Giovanna'
'Nicosia, Carlo'
'Barboza, Tahnie'
'Guy, Laure'
'Dutasta, Jean-Pierre'
'De Zorzi, Rita'
'Demitri, Nicola'
'Dalcanale, Enrico'
'Geremia, Silvano'
_publ_section_title
;
 Enantiospecific recognition of 2-butanol by an inherently chiral cavitand
 in the solid state
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00557A
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'(C55H49O10P3S C4H10O), C4H10O, 0.5 NaBr, H2O'
_chemical_formula_sum            'C63 H71 Br0.5 Na0.5 O13 P3 S'
_chemical_formula_weight         1212.7
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1k2ly5
_audit_creation_date             2017-04-08T11:57:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.769(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7360(10)
_cell_length_b                   21.619(2)
_cell_length_c                   14.974(1)
_cell_measurement_reflns_used    11149
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      1.392
_cell_measurement_wavelength     0.7
_cell_volume                     6257.4(8)
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_molecular_graphics    Pymol
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SIR2011, updated version of SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_av_unetI/netI     0.1223
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            11149
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.392
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.09
_refine_ls_abs_structure_details
;
 Flack x determined using 3188 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.052(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11149
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.062
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0883P)²+0.8327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.165
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                8791
_reflns_number_total             11149
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00557a2.cif
_cod_data_source_block           Rcav_R_2_BuOH
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C63 H71 Br0.50 Na0.50 O13 P3 S'
_cod_database_code               7228320
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.96
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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
O1W O 0.5 0.2464(3) 0.5 0.0126(11) Uiso 1 2 d S . P . .
C1A C 0.1689(4) 0.2141(3) 0.5331(6) 0.0273(16) Uani 1 1 d . . . . .
H1A H 0.1938 0.2107 0.6075 0.033 Uiso 1 1 calc R U . . .
C1B C 0.1362(4) 0.2683(3) 0.4850(6) 0.0287(16) Uani 1 1 d . . . . .
C1C C 0.0989(4) 0.2749(4) 0.3744(6) 0.0296(16) Uani 1 1 d . . . . .
C1D C 0.0951(4) 0.2243(3) 0.3156(6) 0.0263(15) Uani 1 1 d . . . . .
H1D H 0.07 0.2277 0.2412 0.032 Uiso 1 1 calc R U . . .
C1E C 0.1270(4) 0.1679(3) 0.3622(6) 0.0261(15) Uani 1 1 d . . . . .
C1F C 0.1650(4) 0.1640(3) 0.4715(6) 0.0292(16) Uani 1 1 d . . . . .
C1X C 0.1903(4) 0.3985(3) 0.1321(6) 0.0267(15) Uani 1 1 d . . . . .
H1X H 0.2139 0.4374 0.1316 0.032 Uiso 1 1 calc R U . . .
C1Y C 0.1208(4) 0.3959(4) 0.0258(6) 0.0303(17) Uani 1 1 d . . . . .
H1Y1 H 0.1296 0.3878 -0.0313 0.036 Uiso 1 1 calc R U . . .
H1Y2 H 0.0924 0.3615 0.0267 0.036 Uiso 1 1 calc R U . . .
C1Z C 0.0814(5) 0.4564(4) 0.0044(7) 0.0368(19) Uani 1 1 d . . . . .
H1Z1 H 0.0658 0.4609 0.0537 0.055 Uiso 1 1 calc R U . . .
H1Z2 H 0.0413 0.4564 -0.0677 0.055 Uiso 1 1 calc R U . . .
H1Z3 H 0.1119 0.4911 0.0133 0.055 Uiso 1 1 calc R U . . .
C2A C 0.2245(4) 0.4405(3) 0.4041(6) 0.0253(15) Uani 1 1 d . . . . .
H2A H 0.2576 0.4637 0.4635 0.03 Uiso 1 1 calc R U . . .
C2B C 0.2280(4) 0.4367(3) 0.3149(6) 0.0239(15) Uani 1 1 d . . . . .
C2C C 0.1821(4) 0.4027(3) 0.2278(6) 0.0249(15) Uani 1 1 d . . . . .
C2D C 0.1300(4) 0.3705(3) 0.2321(6) 0.0257(15) Uani 1 1 d . . . . .
H2D H 0.0986 0.3457 0.1739 0.031 Uiso 1 1 calc R U . . .
C2E C 0.1227(4) 0.3738(3) 0.3186(6) 0.0259(15) Uani 1 1 d . . . . .
C2F C 0.1707(4) 0.4093(3) 0.4041(6) 0.0240(15) Uani 1 1 d . . . . .
C2Y C 0.1650(4) 0.1658(4) -0.0126(6) 0.0299(16) Uani 1 1 d . . . . .
H2Y1 H 0.1663 0.1915 -0.0663 0.036 Uiso 1 1 calc R U . . .
H2Y2 H 0.1279 0.1819 -0.0033 0.036 Uiso 1 1 calc R U . . .
C2Z C 0.1487(5) 0.0981(4) -0.0514(7) 0.0372(19) Uani 1 1 d . . . . .
H2Z1 H 0.1865 0.0814 -0.0574 0.056 Uiso 1 1 calc R U . . .
H2Z2 H 0.1055 0.0967 -0.1201 0.056 Uiso 1 1 calc R U . . .
H2Z3 H 0.1436 0.0732 -0.0011 0.056 Uiso 1 1 calc R U . . .
C3A C 0.3559(4) 0.3100(4) 0.2123(6) 0.0302(16) Uani 1 1 d . . . . .
H3A H 0.4041 0.3183 0.2464 0.036 Uiso 1 1 calc R U . . .
C3B C 0.3296(4) 0.2508(4) 0.1749(6) 0.0281(15) Uani 1 1 d . . . . .
C3C C 0.2597(4) 0.2369(3) 0.1255(6) 0.0254(15) Uani 1 1 d . . . . .
C3D C 0.2152(4) 0.2853(3) 0.1124(6) 0.0269(15) Uani 1 1 d . . . . .
H3D H 0.1671 0.2769 0.0785 0.032 Uiso 1 1 calc R U . . .
C3E C 0.2383(4) 0.3458(3) 0.1469(6) 0.0259(15) Uani 1 1 d . . . . .
C3F C 0.3100(4) 0.3556(3) 0.1983(6) 0.0276(15) Uani 1 1 d . . . . .
C3Y C 0.0498(4) 0.1041(4) 0.1946(6) 0.0356(18) Uani 1 1 d . . . . .
H3Y1 H 0.0128 0.1106 0.2097 0.043 Uiso 1 1 calc R U . . .
H3Y2 H 0.0448 0.1361 0.1436 0.043 Uiso 1 1 calc R U . . .
C3Z C 0.0418(5) 0.0405(5) 0.1467(8) 0.048(2) Uani 1 1 d . . . . .
H3Z1 H -0.0047 0.0365 0.0841 0.072 Uiso 1 1 calc R U . . .
H3Z2 H 0.0486 0.0088 0.1981 0.072 Uiso 1 1 calc R U . . .
H3Z3 H 0.0764 0.0352 0.1271 0.072 Uiso 1 1 calc R U . . .
C4A C 0.3009(4) 0.0807(4) 0.3473(7) 0.0343(18) Uani 1 1 d . . . . .
H4A H 0.3425 0.061 0.3988 0.041 Uiso 1 1 calc R U . . .
C4B C 0.2440(4) 0.0834(3) 0.3585(7) 0.0324(17) Uani 1 1 d . . . . .
C4C C 0.1828(4) 0.1105(3) 0.2816(6) 0.0285(16) Uani 1 1 d . . . . .
C4D C 0.1797(4) 0.1381(3) 0.1965(6) 0.0262(15) Uani 1 1 d . . . . .
H4D H 0.1382 0.1583 0.1458 0.031 Uiso 1 1 calc R U . . .
C4E C 0.2353(4) 0.1372(3) 0.1826(6) 0.0267(16) Uani 1 1 d . . . . .
C4F C 0.2956(4) 0.1077(3) 0.2588(6) 0.0286(16) Uani 1 1 d . . . . .
C4Y C -0.0017(4) 0.3323(3) 0.2212(6) 0.0283(16) Uani 1 1 d . . . . .
H4Y1 H 0.0056 0.3108 0.1694 0.034 Uiso 1 1 calc R U . . .
H4Y2 H -0.0185 0.3746 0.1943 0.034 Uiso 1 1 calc R U . . .
C4Z C -0.0571(4) 0.2980(4) 0.2299(7) 0.0379(19) Uani 1 1 d . . . . .
H4Z1 H -0.0478 0.2535 0.2355 0.057 Uiso 1 1 calc R U . . .
H4Z2 H -0.1026 0.3063 0.1673 0.057 Uiso 1 1 calc R U . . .
H4Z3 H -0.0565 0.3122 0.2925 0.057 Uiso 1 1 calc R U . . .
C23A C 0.3976(4) 0.5146(4) 0.3429(6) 0.0305(17) Uani 1 1 d . . . . .
C23B C 0.4653(4) 0.5079(4) 0.3712(7) 0.0348(18) Uani 1 1 d . . . . .
H23B H 0.4844 0.4676 0.3806 0.042 Uiso 1 1 calc R U . . .
C23C C 0.5063(5) 0.5589(4) 0.3862(7) 0.0382(19) Uani 1 1 d . . . . .
H23C H 0.5532 0.5535 0.4066 0.046 Uiso 1 1 calc R U . . .
C23D C 0.4789(4) 0.6175(4) 0.3715(7) 0.0348(18) Uani 1 1 d . . . . .
H23D H 0.5069 0.6527 0.382 0.042 Uiso 1 1 calc R U . . .
C23E C 0.4105(4) 0.6248(3) 0.3415(7) 0.0334(18) Uani 1 1 d . . . . .
H23E H 0.3913 0.6652 0.3299 0.04 Uiso 1 1 calc R U . . .
C23F C 0.3697(4) 0.5738(4) 0.3282(7) 0.0355(18) Uani 1 1 d . . . . .
H23F H 0.323 0.5792 0.3093 0.043 Uiso 1 1 calc R U . . .
C34A C 0.4728(4) 0.1175(3) 0.2683(6) 0.0299(17) Uani 1 1 d . . . . .
C34B C 0.4720(4) 0.1154(4) 0.1755(7) 0.0351(18) Uani 1 1 d . . . . .
H34B H 0.4386 0.1387 0.1166 0.042 Uiso 1 1 calc R U . . .
C34C C 0.5196(5) 0.0796(4) 0.1679(7) 0.041(2) Uani 1 1 d . . . . .
H34C H 0.5191 0.0785 0.1041 0.049 Uiso 1 1 calc R U . . .
C34D C 0.5684(4) 0.0451(4) 0.2543(7) 0.0367(19) Uani 1 1 d . . . . .
H34D H 0.6 0.0193 0.2484 0.044 Uiso 1 1 calc R U . . .
C34E C 0.5708(4) 0.0484(4) 0.3475(7) 0.040(2) Uani 1 1 d . . . . .
H34E H 0.6052 0.0261 0.4067 0.048 Uiso 1 1 calc R U . . .
C34F C 0.5232(4) 0.0843(4) 0.3562(7) 0.0386(19) Uani 1 1 d . . . . .
H34F H 0.5248 0.0864 0.4208 0.046 Uiso 1 1 calc R U . . .
C12A C 0.1665(6) 0.4124(4) 0.6671(7) 0.042(2) Uani 1 1 d . . . . .
C12B C 0.0979(6) 0.4240(5) 0.6271(11) 0.060(3) Uani 1 1 d . . . . .
H12B H 0.0655 0.4109 0.5574 0.072 Uiso 1 1 calc R U . . .
C12C C 0.0731(10) 0.4538(5) 0.6822(15) 0.090(5) Uani 1 1 d . . . . .
H12C H 0.0256 0.4639 0.6507 0.108 Uiso 1 1 calc R U . . .
C12D C 0.1231(13) 0.4686(6) 0.7898(16) 0.096(6) Uani 1 1 d . . . . .
H12D H 0.1082 0.4865 0.8325 0.115 Uiso 1 1 calc R U . . .
C12E C 0.1900(15) 0.4576(6) 0.8302(13) 0.105(7) Uani 1 1 d . . . . .
H12E H 0.2223 0.4697 0.9005 0.126 Uiso 1 1 calc R U . . .
C12F C 0.2146(8) 0.4277(5) 0.7702(8) 0.065(3) Uani 1 1 d . . . . .
H12F H 0.2624 0.4189 0.8004 0.078 Uiso 1 1 calc R U . . .
C100 C 0.2600(4) 0.0949(4) 0.5279(6) 0.0314(17) Uani 1 1 d . . . . .
H10A H 0.2815 0.1339 0.5239 0.038 Uiso 1 1 calc R U . . .
H10B H 0.2924 0.0755 0.5966 0.038 Uiso 1 1 calc R U . . .
C2X C 0.2334(4) 0.1707(3) 0.0899(6) 0.0274(16) Uani 1 1 d . . . . .
H2X H 0.2684 0.1497 0.079 0.033 Uiso 1 1 calc R U . . .
C3X C 0.1217(4) 0.1113(4) 0.2980(6) 0.0281(16) Uani 1 1 d . . . . .
H3X H 0.1275 0.0744 0.3423 0.034 Uiso 1 1 calc R U . . .
C4X C 0.0672(4) 0.3371(4) 0.3246(7) 0.0326(17) Uani 1 1 d . . . . .
H4X H 0.0583 0.3595 0.3747 0.039 Uiso 1 1 calc R U . . .
O1A O 0.1377(3) 0.3167(2) 0.5479(4) 0.0300(11) Uani 1 1 d . . . . .
O1B O 0.1974(3) 0.1094(2) 0.5233(4) 0.0297(11) Uani 1 1 d . . . . .
O2A O 0.2793(3) 0.4731(2) 0.3120(4) 0.0277(11) Uani 1 1 d . . . . .
O2B O 0.1623(3) 0.4185(2) 0.4899(4) 0.0296(11) Uani 1 1 d . . . . .
O3A O 0.3780(3) 0.2047(2) 0.1876(4) 0.0292(11) Uani 1 1 d . . . . .
O3B O 0.3363(3) 0.4164(2) 0.2283(4) 0.0308(12) Uani 1 1 d . . . . .
O4A O 0.2512(3) 0.0551(2) 0.4475(4) 0.0324(12) Uani 1 1 d . . . . .
O4B O 0.3521(3) 0.1034(2) 0.2458(4) 0.0328(12) Uani 1 1 d . . . . .
O23 O 0.3852(3) 0.4046(3) 0.4254(5) 0.0387(13) Uani 1 1 d . . . . .
O34 O 0.4308(3) 0.1822(3) 0.3833(5) 0.0407(14) Uani 1 1 d . . . . .
P12 P 0.19191(11) 0.37289(9) 0.58839(16) 0.0288(4) Uani 1 1 d . . . . .
P23 P 0.35127(10) 0.44661(9) 0.33551(16) 0.0274(4) Uani 1 1 d . . . . .
P34 P 0.40878(10) 0.15584(9) 0.28120(16) 0.0299(4) Uani 1 1 d . . . . .
S12 S 0.28664(11) 0.35001(11) 0.65015(19) 0.0441(5) Uani 1 1 d . . . . .
O1I O 0.4497(4) 0.3075(3) 0.5528(7) 0.059(2) Uani 1 1 d . . . . .
H1IA H 0.4413 0.3428 0.5251 0.089 Uiso 1 1 calc R U . . .
C1I C 0.4513(6) 0.2809(6) 0.7124(8) 0.062(3) Uani 1 1 d . . . . .
H1I1 H 0.4844 0.2481 0.724 0.092 Uiso 1 1 calc R U . . .
H1I2 H 0.4208 0.2666 0.7361 0.092 Uiso 1 1 calc R U . . .
H1I3 H 0.4764 0.3178 0.7523 0.092 Uiso 1 1 calc R U . . .
C2I C 0.4074(6) 0.2968(5) 0.5936(9) 0.055(3) Uani 1 1 d . . . . .
H2I H 0.3807 0.3355 0.585 0.066 Uiso 1 1 calc R U . . .
C4I C 0.3040(5) 0.2622(4) 0.4206(8) 0.049(2) Uani 1 1 d . . . . .
H4I1 H 0.278 0.2988 0.4187 0.073 Uiso 1 1 calc R U . . .
H4I2 H 0.2722 0.2272 0.388 0.073 Uiso 1 1 calc R U . . .
H4I3 H 0.3271 0.2707 0.3821 0.073 Uiso 1 1 calc R U . . .
C3I C 0.3574(5) 0.2466(5) 0.5328(9) 0.056(2) Uani 1 1 d . . . . .
H3I1 H 0.3331 0.2349 0.5692 0.067 Uiso 1 1 calc R U . . .
H3I2 H 0.3836 0.2099 0.5333 0.067 Uiso 1 1 calc R U . . .
Na1 Na 0.5 0.2888(12) 0 0.238(9) Uani 1 2 d S T P . .
Br1 Br 0 0.24658(5) 0 0.0396(3) Uani 1 2 d S T P . .
O2W O 0.434(3) 0.369(2) 0.028(4) 0.23(2) Uiso 0.5 1 d . . P . .
O1SA O 0.4241(9) 0.1800(8) -0.0448(13) 0.070(4) Uiso 0.5 1 d D . P A 1
H1SA H 0.4473 0.159 -0.0627 0.106 Uiso 0.5 1 calc R U P A 1
C1SA C 0.3292(16) 0.1275(14) -0.157(2) 0.077(7) Uiso 0.5 1 d . . P A 1
H1S1 H 0.2817 0.1266 -0.2175 0.115 Uiso 0.5 1 calc R U P A 1
H1S2 H 0.3589 0.102 -0.1711 0.115 Uiso 0.5 1 calc R U P A 1
H1S3 H 0.33 0.1111 -0.095 0.115 Uiso 0.5 1 calc R U P A 1
C2SA C 0.354(2) 0.190(4) -0.137(3) 0.22(3) Uiso 0.5 1 d D . P A 1
H2SA H 0.355 0.2084 -0.1972 0.264 Uiso 0.5 1 calc R U P A 1
C3SA C 0.3193(14) 0.2308(13) -0.099(2) 0.153(9) Uiso 0.5 1 d D . P A 1
H3S1 H 0.3616 0.2501 -0.0404 0.184 Uiso 0.5 1 calc R U P A 1
H3S2 H 0.3078 0.1983 -0.0639 0.184 Uiso 0.5 1 calc R U P A 1
C4SA C 0.2675(13) 0.2798(12) -0.106(2) 0.062(6) Uiso 0.5 1 d . . P A 1
H4S1 H 0.2741 0.286 -0.0367 0.094 Uiso 0.5 1 calc R U P A 1
H4S2 H 0.2755 0.319 -0.1313 0.094 Uiso 0.5 1 calc R U P A 1
H4S3 H 0.2202 0.2657 -0.1554 0.094 Uiso 0.5 1 calc R U P A 1
O1SB O 0.3504(13) 0.2544(14) -0.1584(19) 0.120(8) Uiso 0.5 1 d D . P B 2
H1SB H 0.3664 0.2901 -0.137 0.179 Uiso 0.5 1 calc R U P B 2
C1SB C 0.2453(16) 0.2539(15) -0.160(3) 0.088(8) Uiso 0.5 1 d D . P B 2
H1S4 H 0.2445 0.2981 -0.1466 0.133 Uiso 0.5 1 calc R U P B 2
H1S5 H 0.2259 0.2472 -0.2354 0.133 Uiso 0.5 1 calc R U P B 2
H1S6 H 0.2178 0.2312 -0.138 0.133 Uiso 0.5 1 calc R U P B 2
C2SB C 0.317(4) 0.105(2) -0.119(7) 0.25(4) Uiso 0.5 1 d D . P B 2
H2S1 H 0.2807 0.0786 -0.1727 0.371 Uiso 0.5 1 calc R U P B 2
H2S2 H 0.3594 0.1002 -0.1209 0.371 Uiso 0.5 1 calc R U P B 2
H2S3 H 0.3263 0.0937 -0.0498 0.371 Uiso 0.5 1 calc R U P B 2
C2SX C 0.2941(18) 0.1712(15) -0.142(3) 0.093(9) Uiso 0.5 1 d D . P B 2
H2S4 H 0.2817 0.1761 -0.2152 0.112 Uiso 0.5 1 calc R U P B 2
H2S5 H 0.2493 0.1698 -0.1454 0.112 Uiso 0.5 1 calc R U P B 2
C3SX C 0.3193(14) 0.2308(13) -0.099(2) 0.153(9) Uiso 0.5 1 d D . P B 2
H3SX H 0.3462 0.2356 -0.0208 0.184 Uiso 0.5 1 calc R U P B 2
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1B C1A C1F 119.2(7) . .
C1B C1A H1A 120.4 . .
C1F C1A H1A 120.4 . .
C1A C1B O1A 118.1(7) . .
C1A C1B C1C 121.7(7) . .
O1A C1B C1C 120.1(7) . .
C1D C1C C1B 117.7(7) . .
C1D C1C C4X 122.3(7) . .
C1B C1C C4X 120.0(7) . .
C1C C1D C1E 122.1(7) . .
C1C C1D H1D 119 . .
C1E C1D H1D 119 . .
C1F C1E C1D 118.3(7) . .
C1F C1E C3X 119.3(6) . .
C1D C1E C3X 122.5(6) . .
O1B C1F C1E 121.6(7) . .
O1B C1F C1A 117.3(7) . .
C1E C1F C1A 121.0(7) . .
C3E C1X C2C 109.9(6) . .
C3E C1X C1Y 113.0(6) . .
C2C C1X C1Y 113.7(6) . .
C3E C1X H1X 106.6 . .
C2C C1X H1X 106.6 . .
C1Y C1X H1X 106.6 . .
C1Z C1Y C1X 110.7(7) . .
C1Z C1Y H1Y1 109.5 . .
C1X C1Y H1Y1 109.5 . .
C1Z C1Y H1Y2 109.5 . .
C1X C1Y H1Y2 109.5 . .
H1Y1 C1Y H1Y2 108.1 . .
C1Y C1Z H1Z1 109.5 . .
C1Y C1Z H1Z2 109.5 . .
H1Z1 C1Z H1Z2 109.5 . .
C1Y C1Z H1Z3 109.5 . .
H1Z1 C1Z H1Z3 109.5 . .
H1Z2 C1Z H1Z3 109.5 . .
C2B C2A C2F 117.8(7) . .
C2B C2A H2A 121.1 . .
C2F C2A H2A 121.1 . .
C2C C2B C2A 123.2(7) . .
C2C C2B O2A 119.3(6) . .
C2A C2B O2A 117.4(6) . .
C2B C2C C2D 117.2(7) . .
C2B C2C C1X 120.7(6) . .
C2D C2C C1X 122.1(7) . .
C2E C2D C2C 122.3(7) . .
C2E C2D H2D 118.8 . .
C2C C2D H2D 118.8 . .
C2D C2E C2F 117.5(7) . .
C2D C2E C4X 122.2(7) . .
C2F C2E C4X 120.2(6) . .
C2E C2F C2A 121.9(6) . .
C2E C2F O2B 119.8(6) . .
C2A C2F O2B 118.0(6) . .
C2X C2Y C2Z 111.4(7) . .
C2X C2Y H2Y1 109.3 . .
C2Z C2Y H2Y1 109.3 . .
C2X C2Y H2Y2 109.3 . .
C2Z C2Y H2Y2 109.3 . .
H2Y1 C2Y H2Y2 108 . .
C2Y C2Z H2Z1 109.5 . .
C2Y C2Z H2Z2 109.5 . .
H2Z1 C2Z H2Z2 109.5 . .
C2Y C2Z H2Z3 109.5 . .
H2Z1 C2Z H2Z3 109.5 . .
H2Z2 C2Z H2Z3 109.5 . .
C3F C3A C3B 117.8(7) . .
C3F C3A H3A 121.1 . .
C3B C3A H3A 121.1 . .
C3C C3B C3A 122.6(7) . .
C3C C3B O3A 120.7(7) . .
C3A C3B O3A 116.7(6) . .
C3B C3C C3D 117.1(7) . .
C3B C3C C2X 120.9(7) . .
C3D C3C C2X 122.0(7) . .
C3C C3D C3E 123.0(7) . .
C3C C3D H3D 118.5 . .
C3E C3D H3D 118.5 . .
C3D C3E C3F 116.2(7) . .
C3D C3E C1X 123.3(7) . .
C3F C3E C1X 120.5(7) . .
C3A C3F C3E 123.2(7) . .
C3A C3F O3B 117.3(6) . .
C3E C3F O3B 119.2(6) . .
C3Z C3Y C3X 111.2(7) . .
C3Z C3Y H3Y1 109.4 . .
C3X C3Y H3Y1 109.4 . .
C3Z C3Y H3Y2 109.4 . .
C3X C3Y H3Y2 109.4 . .
H3Y1 C3Y H3Y2 108 . .
C3Y C3Z H3Z1 109.5 . .
C3Y C3Z H3Z2 109.5 . .
H3Z1 C3Z H3Z2 109.5 . .
C3Y C3Z H3Z3 109.5 . .
H3Z1 C3Z H3Z3 109.5 . .
H3Z2 C3Z H3Z3 109.5 . .
C4B C4A C4F 118.5(7) . .
C4B C4A H4A 120.7 . .
C4F C4A H4A 120.7 . .
C4C C4B C4A 120.6(7) . .
C4C C4B O4A 122.6(7) . .
C4A C4B O4A 116.7(7) . .
C4D C4C C4B 119.6(7) . .
C4D C4C C3X 122.3(7) . .
C4B C4C C3X 118.1(7) . .
C4C C4D C4E 121.8(7) . .
C4C C4D H4D 119.1 . .
C4E C4D H4D 119.1 . .
C4D C4E C4F 117.7(7) . .
C4D C4E C2X 122.1(7) . .
C4F C4E C2X 120.1(7) . .
C4E C4F C4A 121.8(7) . .
C4E C4F O4B 119.7(7) . .
C4A C4F O4B 118.5(7) . .
C4X C4Y C4Z 113.6(7) . .
C4X C4Y H4Y1 108.8 . .
C4Z C4Y H4Y1 108.8 . .
C4X C4Y H4Y2 108.8 . .
C4Z C4Y H4Y2 108.8 . .
H4Y1 C4Y H4Y2 107.7 . .
C4Y C4Z H4Z1 109.5 . .
C4Y C4Z H4Z2 109.5 . .
H4Z1 C4Z H4Z2 109.5 . .
C4Y C4Z H4Z3 109.5 . .
H4Z1 C4Z H4Z3 109.5 . .
H4Z2 C4Z H4Z3 109.5 . .
C23B C23A C23F 119.4(7) . .
C23B C23A P23 117.6(6) . .
C23F C23A P23 122.9(6) . .
C23A C23B C23C 121.0(8) . .
C23A C23B H23B 119.5 . .
C23C C23B H23B 119.5 . .
C23D C23C C23B 119.9(8) . .
C23D C23C H23C 120.1 . .
C23B C23C H23C 120.1 . .
C23C C23D C23E 119.6(7) . .
C23C C23D H23D 120.2 . .
C23E C23D H23D 120.2 . .
C23D C23E C23F 120.7(7) . .
C23D C23E H23E 119.7 . .
C23F C23E H23E 119.7 . .
C23E C23F C23A 119.4(7) . .
C23E C23F H23F 120.3 . .
C23A C23F H23F 120.3 . .
C34B C34A C34F 120.0(7) . .
C34B C34A P34 123.2(6) . .
C34F C34A P34 116.6(6) . .
C34A C34B C34C 120.2(8) . .
C34A C34B H34B 119.9 . .
C34C C34B H34B 119.9 . .
C34B C34C C34D 119.9(8) . .
C34B C34C H34C 120.1 . .
C34D C34C H34C 120.1 . .
C34E C34D C34C 120.1(8) . .
C34E C34D H34D 120 . .
C34C C34D H34D 120 . .
C34D C34E C34F 120.6(8) . .
C34D C34E H34E 119.7 . .
C34F C34E H34E 119.7 . .
C34E C34F C34A 119.2(8) . .
C34E C34F H34F 120.4 . .
C34A C34F H34F 120.4 . .
C12B C12A C12F 119.7(10) . .
C12B C12A P12 119.4(8) . .
C12F C12A P12 120.8(8) . .
C12A C12B C12C 123.7(14) . .
C12A C12B H12B 118.2 . .
C12C C12B H12B 118.2 . .
C12B C12C C12D 116.4(16) . .
C12B C12C H12C 121.8 . .
C12D C12C H12C 121.8 . .
C12E C12D C12C 120.7(13) . .
C12E C12D H12D 119.6 . .
C12C C12D H12D 119.6 . .
C12D C12E C12F 121.7(17) . .
C12D C12E H12E 119.2 . .
C12F C12E H12E 119.2 . .
C12A C12F C12E 117.7(15) . .
C12A C12F H12F 121.1 . .
C12E C12F H12F 121.1 . .
O4A C100 O1B 113.8(6) . .
O4A C100 H10A 108.8 . .
O1B C100 H10A 108.8 . .
O4A C100 H10B 108.8 . .
O1B C100 H10B 108.8 . .
H10A C100 H10B 107.7 . .
C2Y C2X C3C 115.1(6) . .
C2Y C2X C4E 114.0(6) . .
C3C C2X C4E 107.7(6) . .
C2Y C2X H2X 106.5 . .
C3C C2X H2X 106.5 . .
C4E C2X H2X 106.5 . .
C1E C3X C4C 109.4(6) . .
C1E C3X C3Y 113.7(6) . .
C4C C3X C3Y 113.8(7) . .
C1E C3X H3X 106.4 . .
C4C C3X H3X 106.4 . .
C3Y C3X H3X 106.4 . .
C4Y C4X C1C 114.1(7) . .
C4Y C4X C2E 114.5(6) . .
C1C C4X C2E 107.1(6) . .
C4Y C4X H4X 106.9 . .
C1C C4X H4X 106.9 . .
C2E C4X H4X 106.9 . .
C1B O1A P12 124.3(5) . .
C1F O1B C100 115.8(5) . .
C2B O2A P23 124.0(4) . .
C2F O2B P12 124.0(5) . .
C3B O3A P34 122.2(5) . .
C3F O3B P23 122.0(5) . .
C4B O4A C100 116.3(6) . .
C4F O4B P34 123.4(5) . .
O2B P12 O1A 104.6(3) . .
O2B P12 C12A 100.8(4) . .
O1A P12 C12A 99.3(4) . .
O2B P12 S12 115.3(2) . .
O1A P12 S12 115.6(2) . .
C12A P12 S12 118.7(4) . .
O23 P23 O2A 114.2(3) . .
O23 P23 O3B 113.7(3) . .
O2A P23 O3B 106.0(3) . .
O23 P23 C23A 116.7(4) . .
O2A P23 C23A 102.9(3) . .
O3B P23 C23A 101.9(3) . .
O34 P34 O4B 113.8(3) . .
O34 P34 O3A 114.5(3) . .
O4B P34 O3A 106.1(3) . .
O34 P34 C34A 116.8(4) . .
O4B P34 C34A 101.4(3) . .
O3A P34 C34A 102.7(3) . .
C2I O1I H1IA 109.5 . .
C2I C1I H1I1 109.5 . .
C2I C1I H1I2 109.5 . .
H1I1 C1I H1I2 109.5 . .
C2I C1I H1I3 109.5 . .
H1I1 C1I H1I3 109.5 . .
H1I2 C1I H1I3 109.5 . .
O1I C2I C3I 109.4(9) . .
O1I C2I C1I 111.1(9) . .
C3I C2I C1I 111.3(9) . .
O1I C2I H2I 108.3 . .
C3I C2I H2I 108.3 . .
C1I C2I H2I 108.3 . .
C3I C4I H4I1 109.5 . .
C3I C4I H4I2 109.5 . .
H4I1 C4I H4I2 109.5 . .
C3I C4I H4I3 109.5 . .
H4I1 C4I H4I3 109.5 . .
H4I2 C4I H4I3 109.5 . .
C2I C3I C4I 115.3(9) . .
C2I C3I H3I1 108.5 . .
C4I C3I H3I1 108.5 . .
C2I C3I H3I2 108.5 . .
C4I C3I H3I2 108.5 . .
H3I1 C3I H3I2 107.5 . .
O2W Na1 O2W 91(3) . 2_655
O2W Na1 O1SA 155.3(13) . 2_655
O2W Na1 O1SA 106.2(13) 2_655 2_655
C2SA O1SA H1SA 109.5 . .
C2SA C1SA H1S1 109.5 . .
C2SA C1SA H1S2 109.5 . .
H1S1 C1SA H1S2 109.5 . .
C2SA C1SA H1S3 109.5 . .
H1S1 C1SA H1S3 109.5 . .
H1S2 C1SA H1S3 109.5 . .
C1SA C2SA O1SA 100(4) . .
C1SA C2SA C3SA 114(5) . .
O1SA C2SA C3SA 105(3) . .
C1SA C2SA H2SA 112.2 . .
O1SA C2SA H2SA 112.2 . .
C3SA C2SA H2SA 112.2 . .
C2SA C3SA C4SA 157(3) . .
C2SA C3SA H3S1 97 . .
C4SA C3SA H3S1 97 . .
C2SA C3SA H3S2 97 . .
C4SA C3SA H3S2 97 . .
H3S1 C3SA H3S2 103.5 . .
C3SA C4SA H4S1 109.5 . .
C3SA C4SA H4S2 109.5 . .
H4S1 C4SA H4S2 109.5 . .
C3SA C4SA H4S3 109.5 . .
H4S1 C4SA H4S3 109.5 . .
H4S2 C4SA H4S3 109.5 . .
C3SX O1SB H1SB 109.5 . .
C3SX C1SB H1S4 109.5 . .
C3SX C1SB H1S5 109.5 . .
H1S4 C1SB H1S5 109.5 . .
C3SX C1SB H1S6 109.5 . .
H1S4 C1SB H1S6 109.5 . .
H1S5 C1SB H1S6 109.5 . .
C2SX C2SB H2S1 109.5 . .
C2SX C2SB H2S2 109.5 . .
H2S1 C2SB H2S2 109.5 . .
C2SX C2SB H2S3 109.5 . .
H2S1 C2SB H2S3 109.5 . .
H2S2 C2SB H2S3 109.5 . .
C3SX C2SX C2SB 139(4) . .
C3SX C2SX H2S4 102.3 . .
C2SB C2SX H2S4 102.3 . .
C3SX C2SX H2S5 102.3 . .
C2SB C2SX H2S5 102.3 . .
H2S4 C2SX H2S5 104.9 . .
C2SX C3SX O1SB 104(2) . .
C2SX C3SX C1SB 88(2) . .
O1SB C3SX C1SB 104(2) . .
C2SX C3SX H3SX 118.3 . .
O1SB C3SX H3SX 118.3 . .
C1SB C3SX H3SX 118.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1A C1B 1.372(11) .
C1A C1F 1.395(10) .
C1A H1A 0.95 .
C1B O1A 1.395(9) .
C1B C1C 1.416(11) .
C1C C1D 1.378(11) .
C1C C4X 1.521(11) .
C1D C1E 1.403(11) .
C1D H1D 0.95 .
C1E C1F 1.394(11) .
C1E C3X 1.521(10) .
C1F O1B 1.393(9) .
C1X C3E 1.510(10) .
C1X C2C 1.541(10) .
C1X C1Y 1.545(11) .
C1X H1X 1 .
C1Y C1Z 1.522(10) .
C1Y H1Y1 0.99 .
C1Y H1Y2 0.99 .
C1Z H1Z1 0.98 .
C1Z H1Z2 0.98 .
C1Z H1Z3 0.98 .
C2A C2B 1.381(10) .
C2A C2F 1.397(10) .
C2A H2A 0.95 .
C2B C2C 1.377(10) .
C2B O2A 1.427(9) .
C2C C2D 1.405(10) .
C2D C2E 1.392(10) .
C2D H2D 0.95 .
C2E C2F 1.396(11) .
C2E C4X 1.531(11) .
C2F O2B 1.410(9) .
C2Y C2X 1.507(11) .
C2Y C2Z 1.546(11) .
C2Y H2Y1 0.99 .
C2Y H2Y2 0.99 .
C2Z H2Z1 0.98 .
C2Z H2Z2 0.98 .
C2Z H2Z3 0.98 .
C3A C3F 1.369(11) .
C3A C3B 1.400(11) .
C3A H3A 0.95 .
C3B C3C 1.387(10) .
C3B O3A 1.421(9) .
C3C C3D 1.395(10) .
C3C C2X 1.534(10) .
C3D C3E 1.403(11) .
C3D H3D 0.95 .
C3E C3F 1.405(10) .
C3F O3B 1.417(9) .
C3Y C3Z 1.517(12) .
C3Y C3X 1.558(11) .
C3Y H3Y1 0.99 .
C3Y H3Y2 0.99 .
C3Z H3Z1 0.98 .
C3Z H3Z2 0.98 .
C3Z H3Z3 0.98 .
C4A C4B 1.390(12) .
C4A C4F 1.393(12) .
C4A H4A 0.95 .
C4B C4C 1.386(11) .
C4B O4A 1.396(9) .
C4C C4D 1.374(11) .
C4C C3X 1.534(11) .
C4D C4E 1.387(11) .
C4D H4D 0.95 .
C4E C4F 1.393(11) .
C4E C2X 1.546(10) .
C4F O4B 1.401(9) .
C4Y C4X 1.519(11) .
C4Y C4Z 1.527(11) .
C4Y H4Y1 0.99 .
C4Y H4Y2 0.99 .
C4Z H4Z1 0.98 .
C4Z H4Z2 0.98 .
C4Z H4Z3 0.98 .
C23A C23B 1.373(11) .
C23A C23F 1.393(11) .
C23A P23 1.778(8) .
C23B C23C 1.383(12) .
C23B H23B 0.95 .
C23C C23D 1.377(12) .
C23C H23C 0.95 .
C23D C23E 1.381(12) .
C23D H23D 0.95 .
C23E C23F 1.387(11) .
C23E H23E 0.95 .
C23F H23F 0.95 .
C34A C34B 1.381(12) .
C34A C34F 1.403(12) .
C34A P34 1.773(7) .
C34B C34C 1.382(12) .
C34B H34B 0.95 .
C34C C34D 1.397(13) .
C34C H34C 0.95 .
C34D C34E 1.369(13) .
C34D H34D 0.95 .
C34E C34F 1.392(12) .
C34E H34E 0.95 .
C34F H34F 0.95 .
C12A C12B 1.368(15) .
C12A C12F 1.383(15) .
C12A P12 1.780(8) .
C12B C12C 1.379(16) .
C12B H12B 0.95 .
C12C C12D 1.44(3) .
C12C H12C 0.95 .
C12D C12E 1.33(3) .
C12D H12D 0.95 .
C12E C12F 1.44(2) .
C12E H12E 0.95 .
C12F H12F 0.95 .
C100 O4A 1.405(10) .
C100 O1B 1.424(10) .
C100 H10A 0.99 .
C100 H10B 0.99 .
C2X H2X 1 .
C3X H3X 1 .
C4X H4X 1 .
O1A P12 1.605(5) .
O2A P23 1.588(5) .
O2B P12 1.599(6) .
O3A P34 1.593(6) .
O3B P23 1.595(6) .
O4B P34 1.584(6) .
O23 P23 1.463(6) .
O34 P34 1.451(7) .
P12 S12 1.908(3) .
O1I C2I 1.406(12) .
O1I H1IA 0.84 .
C1I C2I 1.552(16) .
C1I H1I1 0.98 .
C1I H1I2 0.98 .
C1I H1I3 0.98 .
C2I C3I 1.487(16) .
C2I H2I 1 .
C4I C3I 1.504(15) .
C4I H4I1 0.98 .
C4I H4I2 0.98 .
C4I H4I3 0.98 .
C3I H3I1 0.99 .
C3I H3I2 0.99 .
Na1 O2W 2.47(6) .
Na1 O2W 2.47(6) 2_655
Na1 O1SA 2.78(3) 2_655
O1SA C2SA 1.47(3) .
O1SA H1SA 0.84 .
C1SA C2SA 1.43(8) .
C1SA H1S1 0.98 .
C1SA H1S2 0.98 .
C1SA H1S3 0.98 .
C2SA C3SA 1.48(3) .
C2SA H2SA 1 .
C3SA C4SA 1.54(4) .
C3SA H3S1 0.99 .
C3SA H3S2 0.99 .
C4SA H4S1 0.98 .
C4SA H4S2 0.98 .
C4SA H4S3 0.98 .
O1SB C3SX 1.49(2) .
O1SB H1SB 0.84 .
C1SB C3SX 1.51(4) .
C1SB H1S4 0.98 .
C1SB H1S5 0.98 .
C1SB H1S6 0.98 .
C2SB C2SX 1.49(3) .
C2SB H2S1 0.98 .
C2SB H2S2 0.98 .
C2SB H2S3 0.98 .
C2SX C3SX 1.42(4) .
C2SX H2S4 0.99 .
C2SX H2S5 0.99 .
C3SX H3SX 1.0001 .
