#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/00/4510056.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_4510056
loop_
_publ_author_name
'Paul, Mithun'
'Adarsh, N. N.'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Secondary Building Unit (SBU) Controlled Formation of a Catalytically
 Active Metal--Organic Polyhedron (MOP) Derived from a Flexible Tripodal
 Ligand
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1331
_journal_paper_doi               10.1021/cg4018322
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C15 H23 K O10 Zn'
_chemical_formula_sum            'C15 H23 K O10 Zn'
_chemical_formula_weight         467.80
_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                 90.145(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.437(5)
_cell_length_b                   15.985(5)
_cell_length_c                   16.475(6)
_cell_measurement_temperature    293(2)
_cell_volume                     4065(2)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury 3.1'
_computing_publication_material  SHELXTL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi-omega scan'
_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  0.1174
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15532
_diffrn_reflns_theta_full        23.39
_diffrn_reflns_theta_max         23.39
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.9306
_exptl_absorpt_correction_T_min  0.4194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.477
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1916
_reflns_number_gt                1926
_reflns_number_total             2956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4018322_si_002.cif
_cod_data_source_block           y
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4510056
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 0.4555(7) 0.7662(7) -0.1514(5) 0.093(4) Uani 1 1 d .
H1A H 0.4403 0.7186 -0.1839 0.140 Uiso 1 1 calc R
H1B H 0.5174 0.7704 -0.1476 0.140 Uiso 1 1 calc R
H1C H 0.4327 0.8160 -0.1761 0.140 Uiso 1 1 calc R
C2 C 0.4177(5) 0.7563(5) -0.0674(5) 0.052(2) Uani 1 1 d .
C3 C 0.4419(5) 0.8104(5) -0.0039(5) 0.0481(19) Uani 1 1 d .
C4 C 0.5015(6) 0.8816(5) -0.0206(6) 0.070(3) Uani 1 1 d .
H4A H 0.4904 0.9249 0.0194 0.084 Uiso 1 1 calc R
H4B H 0.4866 0.9046 -0.0733 0.084 Uiso 1 1 calc R
C5 C 0.5977(6) 0.8631(6) -0.0200(6) 0.065(2) Uani 1 1 d .
C6 C 0.4429(7) 0.8495(6) 0.1418(6) 0.084(3) Uani 1 1 d .
H6A H 0.4998 0.8701 0.1298 0.126 Uiso 1 1 calc R
H6B H 0.4447 0.8171 0.1909 0.126 Uiso 1 1 calc R
H6C H 0.4040 0.8958 0.1487 0.126 Uiso 1 1 calc R
C7 C 0.4118(5) 0.7956(5) 0.0733(5) 0.0471(19) Uani 1 1 d .
C8 C 0.3549(5) 0.7301(5) 0.0895(4) 0.0448(19) Uani 1 1 d .
C9 C 0.3293(5) 0.6751(4) 0.0255(4) 0.0442(19) Uani 1 1 d .
C10 C 0.3616(5) 0.6898(5) -0.0516(4) 0.048(2) Uani 1 1 d .
C11 C 0.2739(6) 0.6000(6) 0.0435(6) 0.072(3) Uani 1 1 d .
H11A H 0.2801 0.5596 0.0008 0.107 Uiso 1 1 calc R
H11B H 0.2144 0.6168 0.0473 0.107 Uiso 1 1 calc R
H11C H 0.2919 0.5755 0.0941 0.107 Uiso 1 1 calc R
C12 C 0.3382(6) 0.6319(5) -0.1214(5) 0.066(3) Uani 1 1 d .
H12A H 0.2857 0.6017 -0.1076 0.080 Uiso 1 1 calc R
H12B H 0.3261 0.6654 -0.1692 0.080 Uiso 1 1 calc R
C13 C 0.4089(5) 0.5695(5) -0.1412(5) 0.051(2) Uani 1 1 d .
C14 C 0.3790(5) 0.6529(5) 0.2227(4) 0.0469(19) Uani 1 1 d .
C28 C 0.3223(6) 0.7134(5) 0.1754(4) 0.059(2) Uani 1 1 d .
H28A H 0.3196 0.7661 0.2047 0.070 Uiso 1 1 calc R
H28B H 0.2640 0.6910 0.1724 0.070 Uiso 1 1 calc R
O1 O 0.6224(4) 0.7918(3) 0.0020(3) 0.0589(15) Uani 1 1 d .
O2 O 0.6461(4) 0.9215(4) -0.0398(5) 0.097(2) Uani 1 1 d .
O3 O 0.4584(4) 0.5441(3) -0.0903(3) 0.0605(16) Uani 1 1 d .
O4 O 0.4088(4) 0.5466(3) -0.2163(3) 0.0608(16) Uani 1 1 d .
O5 O 0.4315(3) 0.6087(3) 0.1825(3) 0.0414(12) Uani 1 1 d .
O7 O 0.7975(4) 0.8757(3) 0.0091(3) 0.0567(14) Uani 1 1 d .
O8 O 0.7509(4) 0.7396(4) 0.1271(3) 0.0672(16) Uani 1 1 d .
O20 O 0.3697(4) 0.6489(4) 0.2972(3) 0.0657(17) Uani 1 1 d .
O21 O 0.7809(5) 0.9049(5) 0.1796(4) 0.102(2) Uani 1 1 d .
O22 O 0.1962(8) 0.5406(7) 0.2928(7) 0.181(5) Uani 1 1 d .
Zn1 Zn 0.5000 0.46868(7) -0.2500 0.0385(4) Uani 1 2 d S
Zn2 Zn 0.7500 0.7500 0.0000 0.0501(4) Uani 1 2 d S
K1 K 0.46578(11) 0.37244(11) -0.04738(10) 0.0488(7) Uani 1.000(7) 1 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'
Zn Zn 0.2839 1.4301 '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'
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
C10 C2 C3 119.6(7) . .
C10 C2 C1 119.4(8) . .
C3 C2 C1 120.9(8) . .
C10 C2 K1 76.0(4) . 5_665
C3 C2 K1 79.4(4) . 5_665
C1 C2 K1 112.1(5) . 5_665
C7 C3 C2 119.4(7) . .
C7 C3 C4 120.8(8) . .
C2 C3 C4 119.7(8) . .
C7 C3 K1 76.2(4) . 5_665
C2 C3 K1 76.3(4) . 5_665
C4 C3 K1 116.7(5) . 5_665
C3 C4 C5 117.1(7) . .
O2 C5 O1 125.3(9) . .
O2 C5 C4 116.2(8) . .
O1 C5 C4 118.5(8) . .
C3 C7 C8 121.4(7) . .
C3 C7 C6 119.3(8) . .
C8 C7 C6 119.3(8) . .
C3 C7 K1 80.0(4) . 5_665
C8 C7 K1 77.1(4) . 5_665
C6 C7 K1 112.5(5) . 5_665
C7 C8 C9 119.7(7) . .
C7 C8 C28 121.2(7) . .
C9 C8 C28 119.1(7) . .
C7 C8 K1 78.6(4) . 5_665
C9 C8 K1 76.6(4) . 5_665
C28 C8 K1 112.8(4) . 5_665
C10 C9 C8 118.2(7) . .
C10 C9 C11 121.5(7) . .
C8 C9 C11 120.1(7) . .
C10 C9 K1 77.9(4) . 5_665
C8 C9 K1 78.2(4) . 5_665
C11 C9 K1 110.0(5) . 5_665
C9 C10 C2 121.6(7) . .
C9 C10 C12 120.4(8) . .
C2 C10 C12 118.0(8) . .
C9 C10 K1 77.6(4) . 5_665
C2 C10 K1 79.6(4) . 5_665
C12 C10 K1 112.6(4) . 5_665
C13 C12 C10 113.2(6) . .
O3 C13 O4 124.8(7) . .
O3 C13 C12 121.9(7) . .
O4 C13 C12 113.3(6) . .
O20 C14 O5 124.6(6) . .
O20 C14 C28 118.2(7) . .
O5 C14 C28 117.2(6) . .
C14 C28 C8 113.4(6) . .
C5 O1 Zn2 125.0(6) . .
C5 O1 K1 135.8(6) . 5_665
Zn2 O1 K1 98.66(19) . 5_665
C13 O3 K1 121.7(5) . .
C13 O3 K1 130.4(5) . 5_665
K1 O3 K1 103.65(17) . 5_665
C13 O4 Zn1 116.9(5) . .
C14 O5 Zn1 113.6(4) . 5_665
C14 O5 K1 137.2(4) . 5_665
Zn1 O5 K1 102.48(19) 5_665 5_665
Zn2 O7 K1 106.3(2) . 3
C14 O20 K1 143.2(5) . 6_566
O4 Zn1 O4 101.1(4) . 2_654
O4 Zn1 O5 100.0(2) . 6_565
O4 Zn1 O5 128.6(2) 2_654 6_565
O4 Zn1 O5 128.6(2) . 5_665
O4 Zn1 O5 100.0(2) 2_654 5_665
O5 Zn1 O5 102.2(3) 6_565 5_665
O4 Zn1 K1 84.55(16) . .
O4 Zn1 K1 128.40(15) 2_654 .
O5 Zn1 K1 99.77(14) 6_565 .
O5 Zn1 K1 46.36(14) 5_665 .
O4 Zn1 K1 128.40(15) . 2_654
O4 Zn1 K1 84.55(16) 2_654 2_654
O5 Zn1 K1 46.36(14) 6_565 2_654
O5 Zn1 K1 99.77(14) 5_665 2_654
K1 Zn1 K1 131.07(6) . 2_654
O1 Zn2 O1 180.0 . 7_665
O1 Zn2 O8 90.8(2) . .
O1 Zn2 O8 89.2(2) 7_665 .
O1 Zn2 O8 89.2(2) . 7_665
O1 Zn2 O8 90.8(2) 7_665 7_665
O8 Zn2 O8 179.998(1) . 7_665
O1 Zn2 O7 88.8(2) . 7_665
O1 Zn2 O7 91.2(2) 7_665 7_665
O8 Zn2 O7 89.8(2) . 7_665
O8 Zn2 O7 90.2(2) 7_665 7_665
O1 Zn2 O7 91.2(2) . .
O1 Zn2 O7 88.8(2) 7_665 .
O8 Zn2 O7 90.2(2) . .
O8 Zn2 O7 89.8(2) 7_665 .
O7 Zn2 O7 179.999(1) 7_665 .
O1 Zn2 K1 49.89(15) . 5_665
O1 Zn2 K1 130.11(15) 7_665 5_665
O8 Zn2 K1 76.53(16) . 5_665
O8 Zn2 K1 103.47(16) 7_665 5_665
O7 Zn2 K1 42.24(15) 7_665 5_665
O7 Zn2 K1 137.76(15) . 5_665
O1 Zn2 K1 130.11(15) . 3
O1 Zn2 K1 49.89(15) 7_665 3
O8 Zn2 K1 103.47(16) . 3
O8 Zn2 K1 76.53(16) 7_665 3
O7 Zn2 K1 137.76(15) 7_665 3
O7 Zn2 K1 42.24(15) . 3
K1 Zn2 K1 180.0 5_665 3
O5 K1 O7 144.51(15) 5_665 3_445
O5 K1 O3 73.43(15) 5_665 .
O7 K1 O3 91.63(17) 3_445 .
O5 K1 O3 110.67(16) 5_665 5_665
O7 K1 O3 96.11(17) 3_445 5_665
O3 K1 O3 76.35(17) . 5_665
O5 K1 O20 66.63(15) 5_665 6_565
O7 K1 O20 79.91(16) 3_445 6_565
O3 K1 O20 82.92(16) . 6_565
O3 K1 O20 158.80(17) 5_665 6_565
O5 K1 O1 123.39(15) 5_665 5_665
O7 K1 O1 60.89(15) 3_445 5_665
O3 K1 O1 151.18(17) . 5_665
O3 K1 O1 112.75(17) 5_665 5_665
O20 K1 O1 83.70(15) 6_565 5_665
O5 K1 C9 63.65(16) 5_665 5_665
O7 K1 C9 151.29(18) 3_445 5_665
O3 K1 C9 106.87(18) . 5_665
O3 K1 C9 68.28(17) 5_665 5_665
O20 K1 C9 123.22(18) 6_565 5_665
O1 K1 C9 101.82(17) 5_665 5_665
O5 K1 C10 88.08(18) 5_665 5_665
O7 K1 C10 127.08(19) 3_445 5_665
O3 K1 C10 116.74(19) . 5_665
O3 K1 C10 54.52(16) 5_665 5_665
O20 K1 C10 142.83(18) 6_565 5_665
O1 K1 C10 88.84(18) 5_665 5_665
C9 K1 C10 24.43(19) 5_665 5_665
O5 K1 C8 52.99(16) 5_665 5_665
O7 K1 C8 150.74(18) 3_445 5_665
O3 K1 C8 117.53(19) . 5_665
O3 K1 C8 93.25(17) 5_665 5_665
O20 K1 C8 100.32(18) 6_565 5_665
O1 K1 C8 89.94(18) 5_665 5_665
C9 K1 C8 25.12(17) 5_665 5_665
C10 K1 C8 43.14(18) 5_665 5_665
O5 K1 C7 69.80(17) 5_665 5_665
O7 K1 C7 126.60(19) 3_445 5_665
O3 K1 C7 140.8(2) . 5_665
O3 K1 C7 104.29(17) 5_665 5_665
O20 K1 C7 94.54(18) 6_565 5_665
O1 K1 C7 65.71(18) 5_665 5_665
C9 K1 C7 43.48(18) 5_665 5_665
C10 K1 C7 49.80(18) 5_665 5_665
C8 K1 C7 24.35(19) 5_665 5_665
O5 K1 C2 102.49(17) 5_665 5_665
O7 K1 C2 109.18(19) 3_445 5_665
O3 K1 C2 139.7(2) . 5_665
O3 K1 C2 67.68(18) 5_665 5_665
O20 K1 C2 133.4(2) 6_565 5_665
O1 K1 C2 64.43(19) 5_665 5_665
C9 K1 C2 43.2(2) 5_665 5_665
C10 K1 C2 24.45(19) 5_665 5_665
C8 K1 C2 49.98(18) 5_665 5_665
C7 K1 C2 42.48(18) 5_665 5_665
O5 K1 C3 93.10(17) 5_665 5_665
O7 K1 C3 109.31(18) 3_445 5_665
O3 K1 C3 157.14(19) . 5_665
O3 K1 C3 91.94(18) 5_665 5_665
O20 K1 C3 109.08(19) 6_565 5_665
O1 K1 C3 51.59(17) 5_665 5_665
C9 K1 C3 50.28(18) 5_665 5_665
C10 K1 C3 42.82(19) 5_665 5_665
C8 K1 C3 42.56(19) 5_665 5_665
C7 K1 C3 23.80(19) 5_665 5_665
C2 K1 C3 24.29(19) 5_665 5_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.511(11) .
C2 C10 1.398(11) .
C2 C3 1.406(11) .
C2 K1 3.320(7) 5_665
C3 C7 1.376(11) .
C3 C4 1.489(11) .
C3 K1 3.359(7) 5_665
C4 C5 1.514(13) .
C5 O2 1.239(10) .
C5 O1 1.255(10) .
C6 C7 1.498(10) .
C7 C8 1.393(11) .
C7 K1 3.312(7) 5_665
C8 C9 1.428(10) .
C8 C28 1.527(10) .
C8 K1 3.293(7) 5_665
C9 C10 1.386(11) .
C9 C11 1.504(11) .
C9 K1 3.272(7) 5_665
C10 C12 1.517(10) .
C10 K1 3.276(7) 5_665
C12 C13 1.515(11) .
C13 O3 1.204(8) .
C13 O4 1.290(8) .
C14 O20 1.237(8) .
C14 O5 1.264(8) .
C14 C28 1.519(10) .
O1 Zn2 2.081(5) .
O1 K1 3.051(6) 5_665
O3 K1 2.836(6) .
O3 K1 2.878(5) 5_665
O4 Zn1 1.960(5) .
O5 Zn1 1.969(4) 5_665
O5 K1 2.753(5) 5_665
O7 Zn2 2.145(5) .
O7 K1 2.761(6) 3
O8 Zn2 2.101(5) .
O20 K1 2.976(5) 6_566
Zn1 O4 1.960(5) 2_654
Zn1 O5 1.969(4) 6_565
Zn1 O5 1.969(4) 5_665
Zn1 K1 3.715(2) .
Zn1 K1 3.715(2) 2_654
Zn2 O1 2.081(6) 7_665
Zn2 O8 2.101(5) 7_665
Zn2 O7 2.145(5) 7_665
Zn2 K1 3.943(2) 5_665
Zn2 K1 3.943(2) 3
K1 O5 2.753(5) 5_665
K1 O7 2.762(6) 3_445
K1 O3 2.878(5) 5_665
K1 O20 2.976(5) 6_565
K1 O1 3.051(6) 5_665
K1 C9 3.272(7) 5_665
K1 C10 3.276(7) 5_665
K1 C8 3.293(7) 5_665
K1 C7 3.312(7) 5_665
K1 C2 3.320(7) 5_665
K1 C3 3.359(7) 5_665
