#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:31:19 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179533 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/02/4500295.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_4500295
loop_
_publ_author_name
'Lin, Jingxiang'
'Lü, Jian'
'Cao, Minna'
'Cao, Rong'
_publ_section_title
;
 Effects of Cocrystalline Subunits on the Supramolecular Chemistry of
 Me10Q[5]: From Simple Inorganic Anions to Cluster Anions
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              778
_journal_paper_doi               10.1021/cg101355d
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C80 H116 Cl4 K4 N40 O43'
_chemical_formula_weight         2624.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.756(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.5971(13)
_cell_length_b                   17.9071(7)
_cell_length_c                   13.1020(7)
_cell_measurement_temperature    293(2)
_cell_volume                     5197.6(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16017
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6017
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0886P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1558
_reflns_number_gt                3299
_reflns_number_total             6017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101355d_si_003.cif
_cod_data_source_block           c
_cod_original_cell_volume        5197.6(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4500295
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.19577(12) 0.17314(16) -0.1054(3) 0.0246(7) Uani 1 1 d .
H1A H 0.2286 0.1570 -0.1248 0.030 Uiso 1 1 calc R
H1B H 0.2124 0.1746 -0.0217 0.030 Uiso 1 1 calc R
C2 C 0.15965(12) 0.29796(16) -0.0903(2) 0.0227(6) Uani 1 1 d .
C3 C 0.13095(13) 0.42985(16) -0.1005(3) 0.0266(7) Uani 1 1 d .
H3A H 0.1467 0.4231 -0.0175 0.032 Uiso 1 1 calc R
H3B H 0.1515 0.4737 -0.1137 0.032 Uiso 1 1 calc R
C4 C 0.03472(13) 0.42545(15) -0.0889(3) 0.0234(6) Uani 1 1 d .
C5 C -0.03303(12) 0.48943(15) -0.2527(2) 0.0219(6) Uani 1 1 d .
C6 C -0.06045(14) 0.56664(16) -0.2596(3) 0.0331(8) Uani 1 1 d .
H6A H -0.0637 0.5921 -0.3282 0.050 Uiso 1 1 calc R
H6B H -0.0346 0.5959 -0.1928 0.050 Uiso 1 1 calc R
H6C H -0.1007 0.5616 -0.2621 0.050 Uiso 1 1 calc R
C7 C -0.06801(13) 0.43823(15) -0.1056(3) 0.0243(7) Uani 1 1 d .
H7A H -0.0471 0.4359 -0.0219 0.029 Uiso 1 1 calc R
H7B H -0.0958 0.4815 -0.1263 0.029 Uiso 1 1 calc R
C8 C -0.08744(13) 0.30625(16) -0.0848(3) 0.0253(7) Uani 1 1 d .
C9 C -0.15814(12) 0.36348(16) -0.2524(2) 0.0233(6) Uani 1 1 d .
C10 C -0.17715(13) 0.27941(16) -0.2488(3) 0.0239(6) Uani 1 1 d .
C11 C -0.20554(14) 0.42134(18) -0.2618(3) 0.0352(8) Uani 1 1 d .
H11A H -0.1900 0.4715 -0.2634 0.053 Uiso 1 1 calc R
H11B H -0.2147 0.4169 -0.1963 0.053 Uiso 1 1 calc R
H11C H -0.2424 0.4128 -0.3316 0.053 Uiso 1 1 calc R
C12 C -0.23766(14) 0.26933(18) -0.2448(3) 0.0334(8) Uani 1 1 d .
H12A H -0.2696 0.2922 -0.3120 0.050 Uiso 1 1 calc R
H12B H -0.2363 0.2934 -0.1765 0.050 Uiso 1 1 calc R
H12C H -0.2460 0.2159 -0.2432 0.050 Uiso 1 1 calc R
C13 C -0.12324(14) 0.17745(15) -0.1005(3) 0.0261(7) Uani 1 1 d .
H13A H -0.1644 0.1604 -0.1159 0.031 Uiso 1 1 calc R
H13B H -0.0992 0.1793 -0.0172 0.031 Uiso 1 1 calc R
C14 C -0.03702(13) 0.10502(15) -0.0914(2) 0.0211(6) Uani 1 1 d .
C15 C -0.08906(13) -0.05888(16) -0.2487(3) 0.0320(8) Uani 1 1 d .
H15A H -0.0541 -0.0864 -0.2462 0.048 Uiso 1 1 calc R
H15B H -0.1249 -0.0722 -0.3177 0.048 Uiso 1 1 calc R
H15C H -0.0956 -0.0718 -0.1821 0.048 Uiso 1 1 calc R
C16 C -0.07748(12) 0.02488(15) -0.2486(2) 0.0217(6) Uani 1 1 d .
C17 C 0.03526(12) 0.01533(16) -0.1031(3) 0.0235(6) Uani 1 1 d .
H17A H 0.0548 0.0207 -0.0196 0.028 Uiso 1 1 calc R
H17B H 0.0314 -0.0387 -0.1206 0.028 Uiso 1 1 calc R
C18 C 0.11757(12) 0.09824(16) -0.0856(3) 0.0229(6) Uani 1 1 d .
C19 C 0.12902(12) 0.07657(15) -0.2532(2) 0.0223(6) Uani 1 1 d .
C20 C 0.18149(14) 0.03591(17) -0.2610(3) 0.0340(8) Uani 1 1 d .
H20A H 0.1666 0.0072 -0.3316 0.051 Uiso 1 1 calc R
H20B H 0.2003 0.0020 -0.1963 0.051 Uiso 1 1 calc R
H20C H 0.2114 0.0724 -0.2600 0.051 Uiso 1 1 calc R
O1 O 0.15783(9) 0.28648(12) 0.00029(18) 0.0327(5) Uani 1 1 d .
O2 O 0.05446(9) 0.39299(12) 0.00181(18) 0.0317(5) Uani 1 1 d .
O1W O 0.1259(3) 0.2529(2) 0.3030(4) 0.135(2) Uani 1 1 d D
O3 O -0.00070(9) 0.13308(11) -0.00236(18) 0.0312(5) Uani 1 1 d .
O2W O 0.0000 0.2450(9) -0.2500 0.139(5) Uiso 0.50 2 d SPD
O4 O 0.12852(9) 0.12055(12) 0.00966(18) 0.0326(5) Uani 1 1 d .
O3W O 0.0000 0.2174(5) 0.2500 0.170(3) Uiso 1 2 d SD
O5 O -0.04623(10) 0.29933(12) 0.00868(19) 0.0345(5) Uani 1 1 d .
O6 O 0.21520(14) 0.38939(17) 0.3465(2) 0.0676(8) Uani 1 1 d .
O7 O 0.2685(3) 0.4670(3) 0.4953(3) 0.184(3) Uani 1 1 d .
O8 O 0.28302(17) 0.3420(2) 0.5218(3) 0.1090(14) Uani 1 1 d .
O9 O 0.1934(2) 0.3927(4) 0.4989(4) 0.167(3) Uani 1 1 d .
Cl1 Cl 0.24046(5) 0.39670(6) 0.46734(9) 0.0559(3) Uani 1 1 d .
K1 K 0.07498(4) 0.24791(4) 0.07641(8) 0.0489(3) Uani 1 1 d .
N1 N 0.07394(10) 0.04803(13) -0.1475(2) 0.0236(5) Uani 1 1 d .
N2 N -0.02480(10) 0.04763(13) -0.1469(2) 0.0245(5) Uani 1 1 d .
N3 N -0.09615(11) 0.12301(13) -0.1470(2) 0.0248(6) Uani 1 1 d .
N4 N -0.12714(11) 0.25167(13) -0.1452(2) 0.0254(6) Uani 1 1 d .
N5 N -0.10352(11) 0.37094(13) -0.1470(2) 0.0255(6) Uani 1 1 d .
N6 N -0.02324(10) 0.45128(13) -0.1481(2) 0.0238(5) Uani 1 1 d .
N7 N 0.06712(10) 0.44515(13) -0.1469(2) 0.0241(5) Uani 1 1 d .
N8 N 0.14613(11) 0.36415(13) -0.1481(2) 0.0266(6) Uani 1 1 d .
N9 N 0.17749(11) 0.24800(12) -0.1487(2) 0.0246(5) Uani 1 1 d .
N10 N 0.14832(10) 0.11812(13) -0.1474(2) 0.0235(5) Uani 1 1 d .
H2W H 0.0153(12) 0.2491(17) -0.1823(16) 0.028 Uiso 1 1 d D
H1WB H 0.1538(11) 0.2272(17) 0.355(2) 0.028 Uiso 1 1 d D
H3W H 0.0373(9) 0.2349(16) 0.290(2) 0.028 Uiso 1 1 d D
H1WA H 0.1450(13) 0.2906(14) 0.337(3) 0.028 Uiso 1 1 d D
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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
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
N10 C1 N9 114.9(2) . .
O1 C2 N8 125.4(3) . .
O1 C2 N9 126.0(3) . .
N8 C2 N9 108.5(2) . .
N7 C3 N8 114.1(2) . .
O2 C4 N7 125.8(3) . .
O2 C4 N6 126.0(3) . .
N7 C4 N6 108.2(2) . .
N7 C5 N6 113.1(2) 2_554 .
N7 C5 C6 112.1(2) 2_554 .
N6 C5 C6 111.7(2) . .
N7 C5 C5 102.5(2) 2_554 2_554
N6 C5 C5 102.1(2) . 2_554
C6 C5 C5 114.75(16) . 2_554
N5 C7 N6 115.2(2) . .
O5 C8 N4 125.9(3) . .
O5 C8 N5 125.9(3) . .
N4 C8 N5 108.2(3) . .
N5 C9 N8 112.7(2) . 2_554
N5 C9 C11 111.9(2) . .
N8 C9 C11 111.6(2) 2_554 .
N5 C9 C10 102.8(2) . .
N8 C9 C10 102.2(2) 2_554 .
C11 C9 C10 115.0(2) . .
N9 C10 N4 113.0(2) 2_554 .
N9 C10 C12 111.9(2) 2_554 .
N4 C10 C12 111.6(2) . .
N9 C10 C9 102.9(2) 2_554 .
N4 C10 C9 102.1(2) . .
C12 C10 C9 114.8(2) . .
N4 C13 N3 114.2(2) . .
O3 C14 N3 125.6(3) . .
O3 C14 N2 125.2(3) . .
N3 C14 N2 109.1(2) . .
N2 C16 N1 112.6(2) . 2_554
N2 C16 C15 111.5(2) . .
N1 C16 C15 111.4(2) 2_554 .
N2 C16 C19 102.9(2) . 2_554
N1 C16 C19 102.8(2) 2_554 2_554
C15 C16 C19 115.2(2) . 2_554
N1 C17 N2 114.6(2) . .
O4 C18 N1 126.1(3) . .
O4 C18 N10 125.7(3) . .
N1 C18 N10 108.2(2) . .
N10 C19 N3 112.7(2) . 2_554
N10 C19 C20 111.8(2) . .
N3 C19 C20 111.5(2) 2_554 .
N10 C19 C16 102.5(2) . 2_554
N3 C19 C16 102.2(2) 2_554 2_554
C20 C19 C16 115.5(2) . 2_554
C2 O1 K1 138.35(19) . .
C4 O2 K1 137.13(19) . .
C14 O3 K1 141.45(19) . .
C18 O4 K1 128.76(19) . .
C8 O5 K1 130.3(2) . .
O8 Cl1 O9 110.6(3) . .
O8 Cl1 O7 109.0(3) . .
O9 Cl1 O7 110.3(4) . .
O8 Cl1 O6 111.9(2) . .
O9 Cl1 O6 107.8(3) . .
O7 Cl1 O6 107.3(2) . .
O3 K1 O1W 111.55(13) . .
O3 K1 O1 124.29(7) . .
O1W K1 O1 109.54(15) . .
O3 K1 O2 127.13(7) . .
O1W K1 O2 106.76(10) . .
O1 K1 O2 71.34(6) . .
O3 K1 O5 70.75(6) . .
O1W K1 O5 104.77(15) . .
O1 K1 O5 130.48(7) . .
O2 K1 O5 65.18(6) . .
O3 K1 O4 67.36(6) . .
O1W K1 O4 107.51(12) . .
O1 K1 O4 65.50(6) . .
O2 K1 O4 131.54(7) . .
O5 K1 O4 133.99(7) . .
C18 N1 C17 121.1(2) . .
C18 N1 C16 113.0(2) . 2_554
C17 N1 C16 125.4(2) . 2_554
C14 N2 C17 120.7(2) . .
C14 N2 C16 112.6(2) . .
C17 N2 C16 126.7(2) . .
C14 N3 C13 121.0(2) . .
C14 N3 C19 113.1(2) . 2_554
C13 N3 C19 125.4(2) . 2_554
C8 N4 C13 121.4(3) . .
C8 N4 C10 113.2(2) . .
C13 N4 C10 124.8(2) . .
C8 N5 C7 120.6(3) . .
C8 N5 C9 113.3(2) . .
C7 N5 C9 126.1(2) . .
C4 N6 C7 120.2(2) . .
C4 N6 C5 113.4(2) . .
C7 N6 C5 126.4(2) . .
C4 N7 C3 120.5(2) . .
C4 N7 C5 113.5(2) . 2_554
C3 N7 C5 125.5(2) . 2_554
C2 N8 C3 120.7(2) . .
C2 N8 C9 113.2(2) . 2_554
C3 N8 C9 125.5(2) . 2_554
C2 N9 C1 120.4(2) . .
C2 N9 C10 112.9(2) . 2_554
C1 N9 C10 126.6(2) . 2_554
C18 N10 C1 120.9(2) . .
C18 N10 C19 113.1(2) . .
C1 N10 C19 125.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N10 1.441(4) .
C1 N9 1.449(4) .
C2 O1 1.224(3) .
C2 N8 1.367(4) .
C2 N9 1.368(4) .
C3 N7 1.442(4) .
C3 N8 1.454(4) .
C4 O2 1.218(3) .
C4 N7 1.365(4) .
C4 N6 1.374(4) .
C5 N7 1.451(4) 2_554
C5 N6 1.455(4) .
C5 C6 1.524(4) .
C5 C5 1.596(5) 2_554
C7 N5 1.448(4) .
C7 N6 1.452(3) .
C8 O5 1.210(4) .
C8 N4 1.365(4) .
C8 N5 1.372(4) .
C9 N5 1.455(4) .
C9 N8 1.457(4) 2_554
C9 C11 1.524(4) .
C9 C10 1.583(4) .
C10 N9 1.453(4) 2_554
C10 N4 1.467(4) .
C10 C12 1.523(4) .
C13 N4 1.438(3) .
C13 N3 1.455(3) .
C14 O3 1.227(3) .
C14 N3 1.352(4) .
C14 N2 1.365(4) .
C15 C16 1.527(4) .
C16 N2 1.456(4) .
C16 N1 1.462(4) 2_554
C16 C19 1.578(4) 2_554
C17 N1 1.437(3) .
C17 N2 1.453(3) .
C18 O4 1.224(3) .
C18 N1 1.364(4) .
C18 N10 1.374(4) .
C19 N10 1.459(4) .
C19 N3 1.462(4) 2_554
C19 C20 1.524(4) .
C19 C16 1.578(4) 2_554
O1 K1 2.719(2) .
O2 K1 2.744(2) .
O1W K1 2.676(5) .
O3 K1 2.663(2) .
O4 K1 2.950(2) .
O5 K1 2.868(2) .
O6 Cl1 1.434(3) .
O7 Cl1 1.406(5) .
O8 Cl1 1.384(3) .
O9 Cl1 1.391(4) .
N1 C16 1.462(4) 2_554
N3 C19 1.462(4) 2_554
N7 C5 1.451(4) 2_554
N8 C9 1.457(4) 2_554
N9 C10 1.453(4) 2_554
