#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/02/4500294.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_4500294
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            'C40 H50 Cl2 K2 N20 O13.5'
_chemical_formula_weight         1176.1
_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                 116.051(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.4141(9)
_cell_length_b                   17.7598(4)
_cell_length_c                   12.7352(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4960.8(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.845
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10585
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2538
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.205
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0661
_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)+(0.1303P)²+3.5637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                3332
_reflns_number_total             4838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101355d_si_002.cif
_cod_data_source_block           c
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C40H50 Cl2 K2 N20 O13.5'
_cod_database_code               4500294
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
K1 K 0.08041(5) 0.24701(5) 0.09822(10) 0.0425(3) Uani 1 1 d .
Cl1 Cl 0.25518(10) 0.10458(10) 0.52754(17) 0.0863(6) Uani 1 1 d .
O1 O 0.05605(13) 0.39058(14) 0.0054(2) 0.0274(6) Uani 1 1 d .
N1 N 0.17810(15) 0.24921(16) -0.1494(3) 0.0232(7) Uani 1 1 d .
C1 C 0.23891(18) 0.2704(2) -0.2606(4) 0.0315(9) Uani 1 1 d .
H1A H 0.2718 0.2917 -0.1901 0.047 Uiso 1 1 calc R
H1B H 0.2376 0.2961 -0.3297 0.047 Uiso 1 1 calc R
H1C H 0.2463 0.2166 -0.2653 0.047 Uiso 1 1 calc R
O2 O 0.00071(13) 0.13615(14) 0.0014(2) 0.0281(6) Uani 1 1 d .
N2 N 0.14861(15) 0.36714(17) -0.1470(3) 0.0244(7) Uani 1 1 d .
C2 C 0.17820(17) 0.2810(2) -0.2553(3) 0.0213(7) Uani 1 1 d .
O3 O 0.13114(13) 0.12123(15) 0.0176(2) 0.0291(6) Uani 1 1 d .
N3 N 0.06862(15) 0.44735(17) -0.1447(2) 0.0238(7) Uani 1 1 d .
C3 C 0.19768(16) 0.1744(2) -0.1036(3) 0.0218(7) Uani 1 1 d .
H3A H 0.2154 0.1766 -0.0172 0.026 Uiso 1 1 calc R
H3B H 0.2304 0.1583 -0.1248 0.026 Uiso 1 1 calc R
O4 O 0.15845(12) 0.28740(15) 0.0029(2) 0.0285(6) Uani 1 1 d .
N4 N -0.02225(15) 0.45320(16) -0.1442(2) 0.0225(7) Uani 1 1 d .
C4 C 0.16063(16) 0.2995(2) -0.0892(3) 0.0206(7) Uani 1 1 d .
O5 O -0.04445(13) 0.30015(14) 0.0196(2) 0.0295(6) Uani 1 1 d .
N5 N -0.10236(15) 0.37171(16) -0.1420(2) 0.0237(7) Uani 1 1 d .
C5 C 0.13327(18) 0.4331(2) -0.0979(3) 0.0242(8) Uani 1 1 d .
H5A H 0.1499 0.4265 -0.0122 0.029 Uiso 1 1 calc R
H5B H 0.1533 0.4777 -0.1125 0.029 Uiso 1 1 calc R
N6 N -0.12743(14) 0.25243(16) -0.1382(3) 0.0225(7) Uani 1 1 d .
C6 C 0.03575(18) 0.42579(19) -0.0861(3) 0.0205(7) Uani 1 1 d .
N7 N -0.09714(14) 0.12320(16) -0.1440(2) 0.0214(7) Uani 1 1 d .
C7 C -0.03297(17) 0.49283(18) -0.2518(3) 0.0206(8) Uani 1 1 d .
N8 N -0.15000(14) 0.11799(16) -0.3554(2) 0.0217(7) Uani 1 1 d .
C8 C -0.0613(2) 0.5695(2) -0.2598(3) 0.0302(9) Uani 1 1 d .
H8A H -0.0635 0.5959 -0.3291 0.045 Uiso 1 1 calc R
H8B H -0.0364 0.5987 -0.1896 0.045 Uiso 1 1 calc R
H8C H -0.1025 0.5636 -0.2658 0.045 Uiso 1 1 calc R
N9 N -0.02499(14) 0.04709(16) -0.1448(2) 0.0200(6) Uani 1 1 d .
C9 C -0.06708(18) 0.43994(19) -0.0997(3) 0.0227(8) Uani 1 1 d .
H9A H -0.0457 0.4378 -0.0133 0.027 Uiso 1 1 calc R
H9B H -0.0954 0.4833 -0.1212 0.027 Uiso 1 1 calc R
N10 N 0.07524(14) 0.04845(16) -0.1443(2) 0.0203(6) Uani 1 1 d .
C10 C -0.08698(17) 0.30667(19) -0.0770(3) 0.0215(8) Uani 1 1 d .
C11 C -0.15903(17) 0.3658(2) -0.2490(3) 0.0210(7) Uani 1 1 d .
C12 C -0.12376(18) 0.17691(19) -0.0932(3) 0.0229(8) Uani 1 1 d .
H12A H -0.1653 0.1598 -0.1091 0.027 Uiso 1 1 calc R
H12B H -0.0990 0.1778 -0.0074 0.027 Uiso 1 1 calc R
C13 C -0.2053(2) 0.4239(2) -0.2542(4) 0.0326(9) Uani 1 1 d .
H13A H -0.1900 0.4743 -0.2575 0.049 Uiso 1 1 calc R
H13B H -0.2124 0.4196 -0.1844 0.049 Uiso 1 1 calc R
H13C H -0.2437 0.4154 -0.3241 0.049 Uiso 1 1 calc R
C14 C -0.13052(16) 0.07635(19) -0.2467(3) 0.0198(7) Uani 1 1 d .
C15 C -0.18305(19) 0.0353(2) -0.2395(4) 0.0298(9) Uani 1 1 d .
H15A H -0.2119 0.0720 -0.2348 0.045 Uiso 1 1 calc R
H15B H -0.1675 0.0033 -0.1697 0.045 Uiso 1 1 calc R
H15C H -0.2038 0.0040 -0.3093 0.045 Uiso 1 1 calc R
C16 C -0.03679(17) 0.10610(19) -0.0884(3) 0.0193(7) Uani 1 1 d .
C17 C 0.03596(16) 0.0152(2) -0.0993(3) 0.0200(7) Uani 1 1 d .
H17A H 0.0556 0.0206 -0.0132 0.024 Uiso 1 1 calc R
H17B H 0.0323 -0.0394 -0.1172 0.024 Uiso 1 1 calc R
C18 C 0.07796(16) 0.02402(19) -0.2514(3) 0.0186(7) Uani 1 1 d .
C19 C 0.09078(19) -0.06005(19) -0.2474(3) 0.0267(8) Uani 1 1 d .
H19A H 0.0562 -0.0880 -0.2473 0.040 Uiso 1 1 calc R
H19B H 0.1277 -0.0719 -0.1762 0.040 Uiso 1 1 calc R
H19C H 0.0967 -0.0744 -0.3160 0.040 Uiso 1 1 calc R
C20 C 0.11963(16) 0.09857(19) -0.0810(3) 0.0194(7) Uani 1 1 d .
O1W O 0.0000 0.2219(5) 0.2500 0.112(3) Uiso 1 2 d S
O2W O 0.1584(3) 0.2464(3) 0.3647(7) 0.128(3) Uani 1 1 d .
O3W O 0.0000 0.2473(11) -0.2500 0.144(7) Uiso 0.50 2 d SP
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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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
O2 K1 O1 120.56(9) . .
O2 K1 O4 119.54(8) . .
O1 K1 O4 68.48(8) . .
O2 K1 O5 68.83(8) . .
O1 K1 O5 63.79(8) . .
O4 K1 O5 125.65(8) . .
O2 K1 O3 67.14(8) . .
O1 K1 O3 126.46(8) . .
O4 K1 O3 64.40(8) . .
O5 K1 O3 131.38(8) . .
O2 K1 O2W 118.77(12) . .
O1 K1 O2W 112.82(12) . .
O4 K1 O2W 105.83(12) . .
O5 K1 O2W 115.31(12) . .
O3 K1 O2W 103.30(12) . .
O2 K1 O1W 70.90(13) . .
O1 K1 O1W 107.49(15) . .
O4 K1 O1W 169.54(12) . .
O5 K1 O1W 56.62(9) . .
O3 K1 O1W 123.01(16) . .
O2W K1 O1W 66.25(11) . .
C6 O1 K1 143.4(2) . .
C4 N1 C3 120.4(3) . .
C4 N1 C2 113.1(3) . .
C3 N1 C2 126.4(3) . .
C16 O2 K1 147.9(2) . .
C4 N2 C11 113.2(3) . 2_554
C4 N2 C5 120.6(3) . .
C11 N2 C5 126.0(3) 2_554 .
N1 C2 N6 112.0(3) . 2_554
N1 C2 C1 112.8(3) . .
N6 C2 C1 111.0(3) 2_554 .
N1 C2 C11 102.4(3) . 2_554
N6 C2 C11 102.6(3) 2_554 2_554
C1 C2 C11 115.3(3) . 2_554
C20 O3 K1 131.4(2) . .
C6 N3 C5 121.4(3) . .
C6 N3 C7 112.7(3) . 2_554
C5 N3 C7 125.4(3) . 2_554
N1 C3 N8 114.8(3) . 2_554
C4 O4 K1 143.1(2) . .
C6 N4 C9 120.6(3) . .
C6 N4 C7 113.3(3) . .
C9 N4 C7 126.1(3) . .
O4 C4 N1 125.7(3) . .
O4 C4 N2 125.7(3) . .
N1 C4 N2 108.6(3) . .
C10 O5 K1 132.6(2) . .
C10 N5 C9 121.3(3) . .
C10 N5 C11 113.5(3) . .
C9 N5 C11 125.0(3) . .
N3 C5 N2 113.9(3) . .
C10 N6 C12 122.0(3) . .
C10 N6 C2 113.0(3) . 2_554
C12 N6 C2 124.5(3) . 2_554
O1 C6 N4 126.1(3) . .
O1 C6 N3 125.1(4) . .
N4 C6 N3 108.7(3) . .
C16 N7 C12 120.6(3) . .
C16 N7 C14 112.9(3) . .
C12 N7 C14 126.1(3) . .
N4 C7 N3 111.7(3) . 2_554
N4 C7 C8 112.7(3) . .
N3 C7 C8 111.3(3) 2_554 .
N4 C7 C7 102.2(3) . 2_554
N3 C7 C7 102.7(3) 2_554 2_554
C8 C7 C7 115.5(2) . 2_554
C20 N8 C3 121.5(3) 2_554 2_554
C20 N8 C14 113.7(3) 2_554 .
C3 N8 C14 124.8(3) 2_554 .
C16 N9 C18 112.7(3) . 2_554
C16 N9 C17 120.2(3) . .
C18 N9 C17 127.0(3) 2_554 .
N5 C9 N4 114.6(3) . .
C20 N10 C17 121.9(3) . .
C20 N10 C18 113.4(3) . .
C17 N10 C18 124.1(3) . .
O5 C10 N6 126.6(3) . .
O5 C10 N5 125.1(3) . .
N6 C10 N5 108.3(3) . .
N2 C11 N5 112.1(3) 2_554 .
N2 C11 C13 112.1(3) 2_554 .
N5 C11 C13 112.1(3) . .
N2 C11 C2 102.7(3) 2_554 2_554
N5 C11 C2 102.1(3) . 2_554
C13 C11 C2 115.1(3) . 2_554
N6 C12 N7 113.2(3) . .
N8 C14 N7 112.6(3) . .
N8 C14 C15 111.8(3) . .
N7 C14 C15 112.0(3) . .
N8 C14 C18 102.2(3) . 2_554
N7 C14 C18 102.1(3) . 2_554
C15 C14 C18 115.5(3) . 2_554
O2 C16 N7 125.5(3) . .
O2 C16 N9 125.3(3) . .
N7 C16 N9 109.1(3) . .
N10 C17 N9 115.1(3) . .
N9 C18 N10 112.4(3) 2_554 .
N9 C18 C19 113.4(3) 2_554 .
N10 C18 C19 110.7(3) . .
N9 C18 C14 102.9(3) 2_554 2_554
N10 C18 C14 102.0(3) . 2_554
C19 C18 C14 114.7(3) . 2_554
O3 C20 N10 125.9(3) . .
O3 C20 N8 125.8(3) . 2_554
N10 C20 N8 108.3(3) . 2_554
K1 O1W K1 164.6(3) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O2 2.660(3) .
K1 O1 2.763(3) .
K1 O4 2.766(3) .
K1 O5 2.916(3) .
K1 O3 2.949(3) .
K1 O2W 3.077(8) .
K1 O1W 3.3349(16) .
O1 C6 1.219(4) .
N1 C4 1.362(5) .
N1 C3 1.445(5) .
N1 C2 1.464(4) .
C1 C2 1.525(5) .
O2 C16 1.230(4) .
N2 C4 1.371(4) .
N2 C11 1.455(4) 2_554
N2 C5 1.452(5) .
C2 N6 1.469(5) 2_554
C2 C11 1.584(5) 2_554
O3 C20 1.228(4) .
N3 C6 1.369(5) .
N3 C5 1.444(5) .
N3 C7 1.463(4) 2_554
C3 N8 1.448(5) 2_554
O4 C4 1.216(4) .
N4 C6 1.367(5) .
N4 C9 1.456(5) .
N4 C7 1.458(4) .
O5 C10 1.218(4) .
N5 C10 1.374(4) .
N5 C9 1.447(4) .
N5 C11 1.458(5) .
N6 C10 1.354(5) .
N6 C12 1.446(4) .
N6 C2 1.469(5) 2_554
N7 C16 1.359(5) .
N7 C12 1.456(4) .
N7 C14 1.460(4) .
C7 N3 1.463(4) 2_554
C7 C8 1.510(5) .
C7 C7 1.590(7) 2_554
N8 C20 1.361(4) 2_554
N8 C3 1.448(5) 2_554
N8 C14 1.453(4) .
N9 C16 1.370(4) .
N9 C18 1.444(4) 2_554
N9 C17 1.454(5) .
N10 C20 1.360(5) .
N10 C17 1.442(4) .
N10 C18 1.460(4) .
C11 N2 1.455(4) 2_554
C11 C13 1.510(5) .
C11 C2 1.584(5) 2_554
C14 C15 1.513(5) .
C14 C18 1.593(5) 2_554
C18 N9 1.444(4) 2_554
C18 C19 1.522(5) .
C18 C14 1.593(5) 2_554
C20 N8 1.361(4) 2_554
O1W K1 3.3349(16) 2
