# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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data_added_by_encifer
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H5)6 Na2 O Zn3'
_chemical_formula_sum            'C12 H30 Na2 O Zn3'
_chemical_formula_weight         432.45

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'
Na Na 0.0362 0.0249 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_H-M_alt        'P 65 2 2'
_space_group_name_Hall           'P 65 2 (0 0 1)'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+5/6'
'-y, x-y, z+2/3'
'-x, -y, z+1/2'
'-x+y, -x, z+1/3'
'y, -x+y, z+1/6'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'y, x, -z+2/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'

_cell_length_a                   8.7801(5)
_cell_length_b                   8.7801(5)
_cell_length_c                   43.327(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2892.6(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.734
_shelx_estimated_absorpt_T_min   0.604
_shelx_estimated_absorpt_T_max   0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18994
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.679
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2329
_reflns_number_gt                2190
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.549
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+0.8078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2329
_refine_ls_number_parameters     105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0521
_refine_ls_wR_factor_gt          0.0514
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Zn1 Zn 0.50229(5) 0.50229(5) 0.3333 0.03475(12) Uani 1 2 d S T P . .
Zn2 Zn 0.26861(4) 0.04712(4) 0.33846(2) 0.02870(9) Uani 1 1 d . . . . .
Na1 Na 0.30285(16) 0.26030(16) 0.28130(2) 0.0395(3) Uani 1 1 d . . . . .
O1 O 0.2744(3) 0.2744(3) 0.3333 0.0283(5) Uani 1 2 d S T P . .
C1 C 0.5901(5) 0.5819(5) 0.29033(9) 0.0549(9) Uani 1 1 d . . . . .
C2 C 0.7473(7) 0.7681(8) 0.28939(13) 0.118(2) Uani 1 1 d . . . . .
H2A H 0.7123 0.8508 0.2972 0.178 Uiso 1 1 calc R U . . .
H2B H 0.7887 0.7989 0.2681 0.178 Uiso 1 1 calc R U . . .
H2C H 0.8421 0.7744 0.3023 0.178 Uiso 1 1 calc R U . . .
C3 C 0.2733(6) -0.0565(5) 0.29737(8) 0.0473(8) Uani 1 1 d . . . . .
C4 C 0.2521(9) -0.2386(7) 0.29853(10) 0.101(2) Uani 1 1 d . . . . .
H4A H 0.3503 -0.2342 0.3100 0.151 Uiso 1 1 calc R U . . .
H4B H 0.2511 -0.2799 0.2775 0.151 Uiso 1 1 calc R U . . .
H4C H 0.1411 -0.3195 0.3088 0.151 Uiso 1 1 calc R U . . .
C5 C 0.2603(4) -0.0228(4) 0.38307(7) 0.0347(6) Uani 1 1 d . . . . .
C6 C 0.2533(7) -0.1995(5) 0.38515(8) 0.0752(14) Uani 1 1 d . . . . .
H6A H 0.1478 -0.2895 0.3746 0.113 Uiso 1 1 calc R U . . .
H6B H 0.2495 -0.2323 0.4069 0.113 Uiso 1 1 calc R U . . .
H6C H 0.3581 -0.1905 0.3753 0.113 Uiso 1 1 calc R U . . .
H1A H 0.622(6) 0.503(6) 0.2795(10) 0.090 Uiso 1 1 d . U . . .
H1B H 0.497(6) 0.591(6) 0.2794(10) 0.090 Uiso 1 1 d . U . . .
H3A H 0.169(6) -0.066(6) 0.2849(10) 0.090 Uiso 1 1 d . U . . .
H3B H 0.380(6) 0.021(6) 0.2861(11) 0.090 Uiso 1 1 d . U . . .
H5A H 0.161(6) -0.023(6) 0.3920(9) 0.090 Uiso 1 1 d . U . . .
H5B H 0.370(6) 0.067(6) 0.3941(10) 0.090 Uiso 1 1 d . U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.03186(18) 0.03186(18) 0.0362(2) 0.00408(11) -0.00408(11) 0.0127(2)
Zn2 0.03279(17) 0.02979(16) 0.02541(15) -0.00027(12) -0.00299(13) 0.01708(14)
Na1 0.0431(7) 0.0553(7) 0.0236(5) 0.0028(5) -0.0021(5) 0.0272(6)
O1 0.0286(9) 0.0286(9) 0.0264(12) 0.0035(5) -0.0035(5) 0.0133(11)
C1 0.052(2) 0.053(2) 0.050(2) 0.0155(17) 0.0095(17) 0.0191(16)
C2 0.090(4) 0.093(4) 0.085(3) 0.035(3) 0.012(3) -0.019(3)
C3 0.060(2) 0.053(2) 0.0341(16) -0.0108(15) -0.0029(15) 0.0316(18)
C4 0.193(7) 0.082(4) 0.059(2) -0.024(2) -0.010(3) 0.093(4)
C5 0.0462(17) 0.0307(15) 0.0305(14) 0.0033(11) -0.0007(12) 0.0217(14)
C6 0.154(5) 0.058(2) 0.0413(18) 0.0092(18) 0.005(2) 0.074(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.001(3) . ?
Zn1 C1 2.004(4) . ?
Zn1 C1 2.004(4) 9 ?
Zn1 Na1 2.9903(12) 9 ?
Zn2 O1 1.9829(13) . ?
Zn2 C3 2.009(3) . ?
Zn2 C5 2.018(3) . ?
Zn2 Na1 3.0562(12) 9 ?
Na1 O1 2.2784(11) . ?
Na1 C5 2.817(3) 2_554 ?
Na1 C5 2.861(3) 9 ?
Na1 C6 3.037(4) 2_554 ?
Na1 Zn2 3.0563(12) 9 ?
Na1 Na1 4.069(2) 11 ?
Na1 H1A 2.53(5) . ?
Na1 H1B 2.53(5) . ?
Na1 H3A 2.50(4) . ?
Na1 H3B 2.52(4) . ?
O1 Zn2 1.9829(13) 9 ?
O1 Na1 2.2782(11) 9 ?
C1 C2 1.524(6) . ?
C1 H1A 0.98(4) . ?
C1 H1B 0.98(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.515(5) . ?
C3 H3A 1.03(5) . ?
C3 H3B 0.97(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.525(4) . ?
C5 Na1 2.817(3) 6 ?
C5 Na1 2.861(3) 9 ?
C5 H5A 0.96(5) . ?
C5 H5B 1.01(5) . ?
C6 Na1 3.037(4) 6 ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
_geom_angle_publ_flag
O1 Zn1 C1 111.52(12) . . ?
O1 Zn1 C1 111.52(12) . 9 ?
C1 Zn1 C1 137.0(2) . 9 ?
O1 Zn1 Na1 49.60(2) . 9 ?
C1 Zn1 Na1 160.38(12) . 9 ?
C1 Zn1 Na1 62.19(12) 9 9 ?
O1 Zn2 C3 111.12(11) . . ?
O1 Zn2 C5 113.09(9) . . ?
C3 Zn2 C5 135.79(14) . . ?
O1 Zn2 Na1 48.18(2) . 9 ?
C3 Zn2 Na1 159.28(11) . 9 ?
C5 Zn2 Na1 64.92(9) . 9 ?
O1 Na1 C5 168.28(8) . 2_554 ?
O1 Na1 C5 80.15(7) . 9 ?
C5 Na1 C5 88.45(9) 2_554 9 ?
O1 Na1 C6 161.47(9) . 2_554 ?
C5 Na1 C6 29.89(8) 2_554 2_554 ?
C5 Na1 C6 118.32(9) 9 2_554 ?
O1 Na1 Zn2 40.44(4) . 9 ?
C5 Na1 Zn2 128.15(7) 2_554 9 ?
C5 Na1 Zn2 39.72(6) 9 9 ?
C6 Na1 Zn2 158.03(7) 2_554 9 ?
O1 Na1 Na1 123.89(6) . 11 ?
C5 Na1 Na1 44.66(6) 2_554 11 ?
C5 Na1 Na1 43.79(6) 9 11 ?
C6 Na1 Na1 74.54(7) 2_554 11 ?
Zn2 Na1 Na1 83.50(4) 9 11 ?
O1 Na1 H1A 95.2(9) . . ?
C5 Na1 H1A 90.6(10) 2_554 . ?
C5 Na1 H1A 133.2(10) 9 . ?
C6 Na1 H1A 71.4(9) 2_554 . ?
Zn2 Na1 H1A 121.1(10) 9 . ?
Na1 Na1 H1A 119.2(10) 11 . ?
O1 Na1 H1B 90.0(10) . . ?
C5 Na1 H1B 88.4(10) 2_554 . ?
C5 Na1 H1B 95.8(11) 9 . ?
C6 Na1 H1B 86.7(10) 2_554 . ?
Zn2 Na1 H1B 94.4(10) 9 . ?
Na1 Na1 H1B 93.0(11) 11 . ?
H1A Na1 H1B 37.4(15) . . ?
O1 Na1 H3A 89.9(10) . . ?
C5 Na1 H3A 93.9(11) 2_554 . ?
C5 Na1 H3A 95.8(11) 9 . ?
C6 Na1 H3A 89.6(10) 2_554 . ?
Zn2 Na1 H3A 93.2(10) 9 . ?
Na1 Na1 H3A 96.8(11) 11 . ?
H1A Na1 H3A 130.9(16) . . ?
H1B Na1 H3A 168.2(15) . . ?
O1 Na1 H3B 92.7(11) . . ?
C5 Na1 H3B 97.1(11) 2_554 . ?
C5 Na1 H3B 133.0(11) 9 . ?
C6 Na1 H3B 75.9(11) 2_554 . ?
Zn2 Na1 H3B 118.2(11) 9 . ?
Na1 Na1 H3B 124.5(11) 11 . ?
H1A Na1 H3B 93.5(16) . . ?
H1B Na1 H3B 130.8(15) . . ?
H3A Na1 H3B 37.5(14) . . ?
Zn2 O1 Zn2 117.90(13) 9 . ?
Zn2 O1 Zn1 121.05(6) 9 . ?
Zn2 O1 Zn1 121.05(6) . . ?
Zn2 O1 Na1 91.38(4) 9 . ?
Zn2 O1 Na1 90.26(4) . . ?
Zn1 O1 Na1 88.41(7) . . ?
Zn2 O1 Na1 90.26(4) 9 9 ?
Zn2 O1 Na1 91.38(4) . 9 ?
Zn1 O1 Na1 88.41(7) . 9 ?
Na1 O1 Na1 176.81(14) . 9 ?
C2 C1 Zn1 112.5(3) . . ?
C2 C1 H1A 109(3) . . ?
Zn1 C1 H1A 113(3) . . ?
C2 C1 H1B 104(3) . . ?
Zn1 C1 H1B 107(3) . . ?
H1A C1 H1B 111(4) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 Zn2 115.4(3) . . ?
C4 C3 H3A 107(3) . . ?
Zn2 C3 H3A 106(2) . . ?
C4 C3 H3B 109(3) . . ?
Zn2 C3 H3B 111(3) . . ?
H3A C3 H3B 108(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 Zn2 110.1(2) . . ?
C6 C5 Na1 83.09(18) . 6 ?
Zn2 C5 Na1 166.78(14) . 6 ?
C6 C5 Na1 174.3(2) . 9 ?
Zn2 C5 Na1 75.36(9) . 9 ?
Na1 C5 Na1 91.55(9) 6 9 ?
C6 C5 H5A 114(3) . . ?
Zn2 C5 H5A 106(3) . . ?
Na1 C5 H5A 68(3) 6 . ?
Na1 C5 H5A 62(3) 9 . ?
C6 C5 H5B 108(3) . . ?
Zn2 C5 H5B 110(3) . . ?
Na1 C5 H5B 63(3) 6 . ?
Na1 C5 H5B 72(3) 9 . ?
H5A C5 H5B 109(4) . . ?
C5 C6 Na1 67.03(17) . 6 ?
C5 C6 H6A 109.5 . . ?
Na1 C6 H6A 125.6 6 . ?
C5 C6 H6B 109.5 . . ?
Na1 C6 H6B 42.5 6 . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
Na1 C6 H6C 123.1 6 . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_refine_diff_density_max         0.240
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL P6522
CELL 0.71073 8.7801 8.7801 43.3270 90.000 90.000 120.000
ZERR 6.0000 0.0005 0.0005 0.0020 0.000 0.000 0.000
LATT -1
SYMM X-Y, X, 0.833333+Z
SYMM -Y, X-Y, 0.666667+Z
SYMM -X, -Y, 0.5+Z
SYMM -X+Y, -X, 0.333333+Z
SYMM Y, -X+Y, 0.166667+Z
SYMM X-Y, -Y, -Z
SYMM -X, -X+Y, 0.333333-Z
SYMM Y, X, 0.666667-Z
SYMM -Y, -X, 0.166667-Z
SYMM -X+Y, Y, 0.5-Z
SYMM X, X-Y, 0.833333-Z
SFAC C NA O ZN H
UNIT 72 12 6 18 180
MERG 2
FMAP 2
GRID
PLAN 5
EQIV $1 Y,X,2/3-Z
FREE Zn1 Na1
FREE Zn1 Na1_$1
FREE Zn2 Na1
FREE Zn2 Na1_$1
FREE Na1 C1
FREE Na1 C5_$1
FREE Na1 C3
TEMP -100
SIZE 0.15 0.12 0.08
BOND $H
EQIV $1 -X+Y, Y, 0.5-Z
TWIN
L.S. 20
ACTA
WGHT    0.023400    0.807800
BASF   0.02736
FVAR       0.06393
ZN1   4    0.502292    0.502292    0.333333    10.50000    0.03186    0.03186 =
         0.03620    0.00408   -0.00408    0.01269
ZN2   4    0.268612    0.047117    0.338461    11.00000    0.03279    0.02979 =
         0.02541   -0.00027   -0.00299    0.01708
NA1   2    0.302853    0.260296    0.281302    11.00000    0.04308    0.05526 =
         0.02360    0.00279   -0.00210    0.02723
O1    3    0.274355    0.274355    0.333333    10.50000    0.02862    0.02862 =
         0.02641    0.00350   -0.00350    0.01329
C1    1    0.590067    0.581946    0.290329    11.00000    0.05202    0.05326 =
         0.04989    0.01554    0.00954    0.01914
C2    1    0.747323    0.768119    0.289388    11.00000    0.09005    0.09287 =
         0.08547    0.03464    0.01150   -0.01935
AFIX 137
H2A   5    0.712262    0.850766    0.297238    11.00000   -1.50000
H2B   5    0.788731    0.798922    0.268067    11.00000   -1.50000
H2C   5    0.842087    0.774371    0.302255    11.00000   -1.50000
AFIX   0
C3    1    0.273300   -0.056493    0.297372    11.00000    0.05959    0.05299 =
         0.03410   -0.01082   -0.00288    0.03165
C4    1    0.252053   -0.238593    0.298533    11.00000    0.19322    0.08170 =
         0.05929   -0.02437   -0.00953    0.09256
AFIX 137
H4A   5    0.350269   -0.234154    0.310046    11.00000   -1.50000
H4B   5    0.251052   -0.279909    0.277481    11.00000   -1.50000
H4C   5    0.141095   -0.319505    0.308821    11.00000   -1.50000
AFIX   0
C5    1    0.260298   -0.022801    0.383074    11.00000    0.04616    0.03068 =
         0.03049    0.00330   -0.00073    0.02166
C6    1    0.253300   -0.199537    0.385152    11.00000    0.15449    0.05752 =
         0.04131    0.00921    0.00485    0.07380
AFIX 137
H6A   5    0.147806   -0.289473    0.374567    11.00000   -1.50000
H6B   5    0.249491   -0.232273    0.406881    11.00000   -1.50000
H6C   5    0.358105   -0.190467    0.375345    11.00000   -1.50000
AFIX   0
H1A   5    0.621677    0.503289    0.279450    11.00000   -1.20000
H1B   5    0.497380    0.591358    0.279352    11.00000   -1.20000
H3A   5    0.168930   -0.066294    0.284906    11.00000   -1.20000
H3B   5    0.379756    0.020644    0.286084    11.00000   -1.20000
H5A   5    0.160685   -0.022539    0.392044    11.00000   -1.20000
H5B   5    0.370078    0.066609    0.394054    11.00000   -1.20000
HKLF 4  1  -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000

REM  P6522
REM R1 =  0.0230 for    2190 Fo > 4sig(Fo)  and  0.0257 for all    2329 data
REM    105 parameters refined using      0 restraints

END

WGHT      0.0222      0.7482

REM Highest difference peak  0.240,  deepest hole -0.346,  1-sigma level  0.079
Q1    1   0.3573 -0.3250  0.4099  11.00000  0.05    0.19
Q2    1   0.3511 -0.2978  0.2500  10.50000  0.05    0.19
Q3    1   0.7508  0.8776  0.2505  11.00000  0.05    0.18
Q4    1   0.2668 -0.0084  0.3133  11.00000  0.05    0.18
Q5    1   0.1148 -0.2902  0.4070  11.00000  0.05    0.18
;
_shelx_res_checksum              82874
_database_code_depnum_ccdc_archive 'CCDC 988444'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_added_by_encifer
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2 H5)8 K2 O Zn4'
_chemical_formula_sum            'C16 H40 K2 O Zn4'
_chemical_formula_weight         588.16

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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   9.0272(18)
_cell_length_b                   9.0272(18)
_cell_length_c                   14.145(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1152.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_F_000             604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    4.473
_shelx_estimated_absorpt_T_min   0.347
_shelx_estimated_absorpt_T_max   0.453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_T_max  0.454
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5225
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.677
_diffrn_reflns_theta_max         28.138
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             697
_reflns_number_gt                483
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0167P)²+0.5855P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         697
_refine_ls_number_parameters     30
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0430
_refine_ls_wR_factor_gt          0.0380
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Zn1 Zn 0.41377(2) 0.08623(2) 0.2500 0.01353(10) Uani 1 2 d S T P . .
K1 K 0.2500 0.2500 0.44908(6) 0.01830(18) Uani 1 4 d S T P . .
O1 O 0.2500 0.2500 0.2500 0.0127(7) Uani 1 8 d S T P . .
C1 C 0.3945(2) -0.0308(2) 0.37015(15) 0.0166(4) Uani 1 1 d . . . . .
H1A H 0.4412 0.0272 0.4215 0.020 Uiso 1 1 calc R U . . .
H1B H 0.2877 -0.0387 0.3853 0.020 Uiso 1 1 calc R U . . .
C2 C 0.4603(3) -0.1872(2) 0.37267(17) 0.0231(5) Uani 1 1 d . . . . .
H2A H 0.4031 -0.2522 0.3308 0.035 Uiso 1 1 calc R U . . .
H2B H 0.4563 -0.2256 0.4374 0.035 Uiso 1 1 calc R U . . .
H2C H 0.5635 -0.1839 0.3513 0.035 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01366(12) 0.01366(12) 0.01328(16) 0.00172(14) 0.00172(14) 0.00076(10)
K1 0.0197(2) 0.0197(2) 0.0155(4) 0.000 0.000 0.000
O1 0.0131(10) 0.0131(10) 0.0120(17) 0.000 0.000 0.000
C1 0.0177(10) 0.0166(10) 0.0154(10) 0.0006(9) 0.0005(9) 0.0005(8)
C2 0.0305(12) 0.0182(10) 0.0207(12) 0.0040(9) -0.0007(10) 0.0029(10)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 C1 2.009(2) 8 ?
Zn1 C1 2.009(2) . ?
Zn1 O1 2.0908(5) . ?
Zn1 Zn1 2.9568(7) 4 ?
Zn1 Zn1 2.9568(7) 2 ?
Zn1 K1 3.5072(8) . ?
Zn1 K1 3.5072(8) 5 ?
K1 O1 2.8159(10) . ?
K1 Zn1 3.5072(8) 4 ?
K1 Zn1 3.5072(8) 3 ?
K1 Zn1 3.5072(8) 2 ?
O1 Zn1 2.0908(5) 4 ?
O1 Zn1 2.0908(5) 2 ?
O1 Zn1 2.0908(5) 3 ?
O1 K1 2.8159(10) 5 ?
C1 C2 1.532(3) . ?

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
_geom_angle_publ_flag
C1 Zn1 C1 143.82(12) 8 . ?
C1 Zn1 O1 108.09(6) 8 . ?
C1 Zn1 O1 108.09(6) . . ?
C1 Zn1 Zn1 121.73(6) 8 4 ?
C1 Zn1 Zn1 85.02(6) . 4 ?
O1 Zn1 Zn1 45.0 . 4 ?
C1 Zn1 Zn1 85.02(6) 8 2 ?
C1 Zn1 Zn1 121.73(6) . 2 ?
O1 Zn1 Zn1 45.0 . 2 ?
Zn1 Zn1 Zn1 90.0 4 2 ?
C1 Zn1 K1 149.82(6) 8 . ?
C1 Zn1 K1 60.38(6) . . ?
O1 Zn1 K1 53.406(11) . . ?
Zn1 Zn1 K1 65.069(7) 4 . ?
Zn1 Zn1 K1 65.069(7) 2 . ?
C1 Zn1 K1 60.38(6) 8 5 ?
C1 Zn1 K1 149.82(6) . 5 ?
O1 Zn1 K1 53.407(12) . 5 ?
Zn1 Zn1 K1 65.069(7) 4 5 ?
Zn1 Zn1 K1 65.069(7) 2 5 ?
K1 Zn1 K1 106.81(2) . 5 ?
O1 K1 Zn1 36.594(11) . . ?
O1 K1 Zn1 36.594(11) . 4 ?
Zn1 K1 Zn1 49.863(14) . 4 ?
O1 K1 Zn1 36.594(11) . 3 ?
Zn1 K1 Zn1 73.19(2) . 3 ?
Zn1 K1 Zn1 49.863(14) 4 3 ?
O1 K1 Zn1 36.594(12) . 2 ?
Zn1 K1 Zn1 49.863(14) . 2 ?
Zn1 K1 Zn1 73.19(2) 4 2 ?
Zn1 K1 Zn1 49.863(14) 3 2 ?
Zn1 O1 Zn1 90.0 . 4 ?
Zn1 O1 Zn1 90.0 . 2 ?
Zn1 O1 Zn1 180.0 4 2 ?
Zn1 O1 Zn1 180.0 . 3 ?
Zn1 O1 Zn1 90.0 4 3 ?
Zn1 O1 Zn1 90.0 2 3 ?
Zn1 O1 K1 90.0 . . ?
Zn1 O1 K1 90.0 4 . ?
Zn1 O1 K1 90.0 2 . ?
Zn1 O1 K1 90.0 3 . ?
Zn1 O1 K1 90.0 . 5 ?
Zn1 O1 K1 90.0 4 5 ?
Zn1 O1 K1 90.0 2 5 ?
Zn1 O1 K1 90.0 3 5 ?
K1 O1 K1 180.0 . 5 ?
C2 C1 Zn1 118.08(16) . . ?

_refine_diff_density_max         0.459
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.069

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL P4nnc in P4/nnc
CELL 0.71073 9.0272 9.0272 14.1446 90.000 90.000 90.000
ZERR 2.0000 0.0018 0.0018 0.0028 0.000 0.000 0.000
LATT 1
SYMM 0.5-Y, X, Z
SYMM 0.5-X, 0.5-Y, Z
SYMM Y, 0.5-X, Z
SYMM X, 0.5-Y, 0.5-Z
SYMM 0.5-X, Y, 0.5-Z
SYMM Y, X, 0.5-Z
SYMM 0.5-Y, 0.5-X, 0.5-Z
SFAC C H O K ZN
UNIT 32 80 2 4 8
MERG 2
FMAP
GRID
PLAN
EQIV $1 1/2-X,1/2-Y,Z
EQIV $2 Y,1/2-X,Z
EQIV $3 1/2-Y,X,Z
FREE K1 C1
FREE K1 C1_$1
FREE K1 C1_$2
FREE K1 C1_$3
TEMP -100
SIZE 0.21 0.28 0.3
L.S. 20
ACTA
WGHT    0.016700    0.585500
FVAR       0.13289
ZN1   5    0.413770    0.086230    0.250000    10.50000    0.01366    0.01366 =
         0.01328    0.00172    0.00172    0.00076
K1    4    0.250000    0.250000    0.449077    10.25000    0.01971    0.01971 =
         0.01547    0.00000    0.00000    0.00000
O1    3    0.250000    0.250000    0.250000    10.12500    0.01310    0.01310 =
         0.01197    0.00000    0.00000    0.00000
C1    1    0.394465   -0.030789    0.370153    11.00000    0.01773    0.01660 =
         0.01542    0.00056    0.00053    0.00050
AFIX  23
H1A   2    0.441199    0.027248    0.421507    11.00000   -1.20000
H1B   2    0.287686   -0.038741    0.385284    11.00000   -1.20000
AFIX   0
C2    1    0.460259   -0.187234    0.372665    11.00000    0.03048    0.01818 =
         0.02074    0.00402   -0.00070    0.00292
AFIX 137
H2A   2    0.403075   -0.252199    0.330840    11.00000   -1.50000
H2B   2    0.456281   -0.225621    0.437424    11.00000   -1.50000
H2C   2    0.563496   -0.183925    0.351339    11.00000   -1.50000
AFIX   0
HKLF 4

REM  P4nnc in P4/nnc
REM R1 =  0.0185 for     483 Fo > 4sig(Fo)  and  0.0361 for all     697 data
REM     30 parameters refined using      0 restraints

END

WGHT      0.0165      0.6104

REM Highest difference peak  0.459,  deepest hole -0.224,  1-sigma level  0.069
Q1    1   0.4129  0.0111  0.3225  11.00000  0.05    0.46
Q2    1   0.4654  0.0869  0.3138  11.00000  0.05    0.34
Q3    1   0.4233 -0.0978  0.3705  11.00000  0.05    0.29
Q4    1   0.3622  0.0961  0.3169  11.00000  0.05    0.27
Q5    1   0.3352  0.1946  0.2566  11.00000  0.05    0.25
Q6    1   0.5006  0.1506  0.2507  11.00000  0.05    0.23
Q7    1   0.4859  0.0141  0.2500  10.50000  0.05    0.21
Q8    1   0.6327 -0.2054  0.3724  11.00000  0.05    0.21
Q9    1   0.3799  0.0713  0.4412  11.00000  0.05    0.20
Q10   1   0.4021  0.0945  0.3566  11.00000  0.05    0.20
Q11   1   0.2825 -0.2520  0.3308  11.00000  0.05    0.19
Q12   1   0.4453 -0.2502  0.4196  11.00000  0.05    0.19
Q13   1   0.3863  0.0005  0.3998  11.00000  0.05    0.19
Q14   1   0.2979  0.0811  0.3735  11.00000  0.05    0.18
Q15   1   0.2500  0.2500  0.3067  10.25000  0.05    0.18
Q16   1   0.4487 -0.2182  0.3410  11.00000  0.05    0.18
Q17   1   0.4223 -0.2498  0.4799  11.00000  0.05    0.17
Q18   1   0.4877 -0.2912  0.2955  11.00000  0.05    0.17
Q19   1   0.3983 -0.2869  0.4301  11.00000  0.05    0.17
Q20   1   0.6072 -0.1706  0.3801  11.00000  0.05    0.17
;
_shelx_res_checksum              37270
_database_code_depnum_ccdc_archive 'CCDC 988445'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_added_by_encifer
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C2H5)8 Rb2 O Zn4'
_chemical_formula_sum            'C16 H40 O Rb2 Zn4'
_chemical_formula_weight         680.90

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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   9.446(3)
_cell_length_b                   9.446(3)
_cell_length_c                   14.199(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1266.8(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_F_000             676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    7.559
_shelx_estimated_absorpt_T_min   0.103
_shelx_estimated_absorpt_T_max   0.210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_T_max  0.210
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7169
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.590
_diffrn_reflns_theta_max         28.208
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             774
_reflns_number_gt                378
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0424P)²+3.1418P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         774
_refine_ls_number_parameters     30
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1317
_refine_ls_wR_factor_gt          0.1055
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Rb1 Rb 0.2500 0.2500 0.53958(8) 0.0991(6) Uani 1 4 d S T P . .
Zn1 Zn 0.09478(8) 0.09478(8) 0.7500 0.0776(4) Uani 1 2 d S T P . .
O1 O 0.2500 0.2500 0.7500 0.073(3) Uani 1 8 d S T P . .
C1 C 0.1153(11) -0.0340(9) 0.6383(6) 0.132(4) Uani 1 1 d . . . . .
H1A H 0.1008 0.0233 0.5824 0.159 Uiso 1 1 calc R U . . .
H1B H 0.2131 -0.0655 0.6369 0.159 Uiso 1 1 calc R U . . .
C2 C 0.0329(12) -0.1509(10) 0.6291(6) 0.142(4) Uani 1 1 d . . . . .
H2A H 0.0393 -0.2071 0.6853 0.213 Uiso 1 1 calc R U . . .
H2B H 0.0647 -0.2056 0.5762 0.213 Uiso 1 1 calc R U . . .
H2C H -0.0637 -0.1227 0.6193 0.213 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rb1 0.1242(8) 0.1242(8) 0.0490(6) 0.000 0.000 0.000
Zn1 0.0901(6) 0.0901(6) 0.0526(5) -0.0104(4) 0.0104(4) -0.0062(5)
O1 0.083(5) 0.083(5) 0.054(6) 0.000 0.000 0.000
C1 0.182(9) 0.114(7) 0.101(6) -0.042(6) 0.038(6) -0.041(7)
C2 0.179(9) 0.154(9) 0.094(6) -0.031(6) -0.022(6) -0.026(9)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O1 2.9876(15) . ?
Rb1 C1 3.283(9) 2 ?
Rb1 Zn1 3.6367(14) 3 ?
Rb1 Zn1 3.6367(14) 4 ?
Rb1 Zn1 3.6367(14) 2 ?
Rb1 Zn1 3.6367(14) . ?
Rb1 C2 3.708(9) 9_556 ?
Rb1 C2 3.708(9) 10_656 ?
Rb1 C2 3.708(9) 11_666 ?
Rb1 C2 3.708(9) 12_566 ?
Zn1 C1 2.008(7) 7_556 ?
Zn1 C1 2.008(7) . ?
Zn1 O1 2.0736(12) . ?
Zn1 Zn1 2.9324(17) 4 ?
Zn1 Zn1 2.9324(17) 2 ?
Zn1 Rb1 3.6367(14) 5_556 ?
O1 Zn1 2.0735(12) 3 ?
O1 Zn1 2.0735(12) 4 ?
O1 Zn1 2.0735(12) 2 ?
O1 Rb1 2.9876(15) 5_556 ?
C1 C2 1.358(10) . ?

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
_geom_angle_publ_flag
O1 Rb1 C1 64.73(14) . 2 ?
O1 Rb1 Zn1 34.76(2) . 3 ?
C1 Rb1 Zn1 58.41(18) 2 3 ?
O1 Rb1 Zn1 34.76(2) . 4 ?
C1 Rb1 Zn1 97.76(15) 2 4 ?
Zn1 Rb1 Zn1 47.55(3) 3 4 ?
O1 Rb1 Zn1 34.76(2) . 2 ?
C1 Rb1 Zn1 33.25(13) 2 2 ?
Zn1 Rb1 Zn1 47.55(3) 3 2 ?
Zn1 Rb1 Zn1 69.52(4) 4 2 ?
O1 Rb1 Zn1 34.76(2) . . ?
C1 Rb1 Zn1 79.78(13) 2 . ?
Zn1 Rb1 Zn1 69.52(4) 3 . ?
Zn1 Rb1 Zn1 47.55(3) 4 . ?
Zn1 Rb1 Zn1 47.55(3) 2 . ?
O1 Rb1 C2 130.23(16) . 9_556 ?
C1 Rb1 C2 140.1(2) 2 9_556 ?
Zn1 Rb1 C2 157.35(16) 3 9_556 ?
Zn1 Rb1 C2 109.99(16) 4 9_556 ?
Zn1 Rb1 C2 136.00(15) 2 9_556 ?
Zn1 Rb1 C2 97.96(16) . 9_556 ?
O1 Rb1 C2 130.23(16) . 10_656 ?
C1 Rb1 C2 77.9(2) 2 10_656 ?
Zn1 Rb1 C2 136.00(15) 3 10_656 ?
Zn1 Rb1 C2 157.35(16) 4 10_656 ?
Zn1 Rb1 C2 97.96(16) 2 10_656 ?
Zn1 Rb1 C2 109.99(16) . 10_656 ?
C2 Rb1 C2 65.34(17) 9_556 10_656 ?
O1 Rb1 C2 130.23(16) . 11_666 ?
C1 Rb1 C2 77.57(18) 2 11_666 ?
Zn1 Rb1 C2 97.96(16) 3 11_666 ?
Zn1 Rb1 C2 136.00(15) 4 11_666 ?
Zn1 Rb1 C2 109.99(16) 2 11_666 ?
Zn1 Rb1 C2 157.35(16) . 11_666 ?
C2 Rb1 C2 99.5(3) 9_556 11_666 ?
C2 Rb1 C2 65.34(17) 10_656 11_666 ?
O1 Rb1 C2 130.23(16) . 12_566 ?
C1 Rb1 C2 139.56(18) 2 12_566 ?
Zn1 Rb1 C2 109.99(16) 3 12_566 ?
Zn1 Rb1 C2 97.96(15) 4 12_566 ?
Zn1 Rb1 C2 157.35(16) 2 12_566 ?
Zn1 Rb1 C2 136.00(15) . 12_566 ?
C2 Rb1 C2 65.34(17) 9_556 12_566 ?
C2 Rb1 C2 99.5(3) 10_656 12_566 ?
C2 Rb1 C2 65.34(17) 11_666 12_566 ?
C1 Zn1 C1 137.8(5) 7_556 . ?
C1 Zn1 O1 111.1(3) 7_556 . ?
C1 Zn1 O1 111.1(3) . . ?
C1 Zn1 Zn1 84.5(3) 7_556 4 ?
C1 Zn1 Zn1 127.3(3) . 4 ?
O1 Zn1 Zn1 45.0 . 4 ?
C1 Zn1 Zn1 127.3(3) 7_556 2 ?
C1 Zn1 Zn1 84.4(3) . 2 ?
O1 Zn1 Zn1 45.0 . 2 ?
Zn1 Zn1 Zn1 90.0 4 2 ?
C1 Zn1 Rb1 63.7(3) 7_556 5_556 ?
C1 Zn1 Rb1 148.7(3) . 5_556 ?
O1 Zn1 Rb1 55.24(2) . 5_556 ?
Zn1 Zn1 Rb1 66.223(13) 4 5_556 ?
Zn1 Zn1 Rb1 66.223(13) 2 5_556 ?
C1 Zn1 Rb1 148.7(3) 7_556 . ?
C1 Zn1 Rb1 63.7(3) . . ?
O1 Zn1 Rb1 55.24(2) . . ?
Zn1 Zn1 Rb1 66.223(13) 4 . ?
Zn1 Zn1 Rb1 66.223(13) 2 . ?
Rb1 Zn1 Rb1 110.47(4) 5_556 . ?
Zn1 O1 Zn1 90.0 3 4 ?
Zn1 O1 Zn1 90.0 3 2 ?
Zn1 O1 Zn1 180.0 4 2 ?
Zn1 O1 Zn1 180.0 3 . ?
Zn1 O1 Zn1 90.0 4 . ?
Zn1 O1 Zn1 90.0 2 . ?
Zn1 O1 Rb1 90.0 3 5_556 ?
Zn1 O1 Rb1 90.0 4 5_556 ?
Zn1 O1 Rb1 90.0 2 5_556 ?
Zn1 O1 Rb1 90.0 . 5_556 ?
Zn1 O1 Rb1 90.0 3 . ?
Zn1 O1 Rb1 90.0 4 . ?
Zn1 O1 Rb1 90.0 2 . ?
Zn1 O1 Rb1 90.0 . . ?
Rb1 O1 Rb1 180.0 5_556 . ?
C2 C1 Zn1 120.8(7) . . ?

_refine_diff_density_max         0.544
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.075

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL p4_nnc in P4/nnc
CELL 0.71073 9.4458 9.4458 14.1986 90.000 90.000 90.000
ZERR 2.0000 0.0030 0.0030 0.0046 0.000 0.000 0.000
LATT 1
SYMM 0.5-Y, X, Z
SYMM 0.5-X, 0.5-Y, Z
SYMM Y, 0.5-X, Z
SYMM X, 0.5-Y, 0.5-Z
SYMM 0.5-X, Y, 0.5-Z
SYMM Y, X, 0.5-Z
SYMM 0.5-Y, 0.5-X, 0.5-Z
SFAC C H O ZN RB
UNIT 32 80 2 8 4
MERG 2
FMAP
GRID
PLAN
EQIV $1 1/2-Y,X,Z
EQIV $2 1/2-X,1/2-Y,Z
EQIV $3 Y,1/2-X,Z
FREE Rb1 C1
FREE Rb1 C1_$1
FREE Rb1 C1_$2
FREE Rb1 C1_$3
TEMP -13
SIZE 0.3 0.35 0.55
EQIV $1 -X, -Y, 1-Z
FREE C2 RB1_$1
L.S. 20
ACTA
WGHT    0.042400    3.141800
FVAR       0.14948
RB1   5    0.250000    0.250000    0.539585    10.25000    0.12422    0.12422 =
         0.04899    0.00000    0.00000    0.00000
ZN1   4    0.094775    0.094775    0.750000    10.50000    0.09014    0.09014 =
         0.05258   -0.01040    0.01040   -0.00618
O1    3    0.250000    0.250000    0.750000    10.12500    0.08300    0.08300 =
         0.05365    0.00000    0.00000    0.00000
C1    1    0.115341   -0.033999    0.638275    11.00000    0.18167    0.11375 =
         0.10105   -0.04183    0.03813   -0.04094
AFIX  23
H1A   2    0.100804    0.023295    0.582411    11.00000   -1.20000
H1B   2    0.213051   -0.065522    0.636862    11.00000   -1.20000
AFIX   0
C2    1    0.032859   -0.150925    0.629117    11.00000    0.17909    0.15359 =
         0.09381   -0.03135   -0.02202   -0.02600
AFIX 137
H2A   2    0.039284   -0.207054    0.685320    11.00000   -1.50000
H2B   2    0.064655   -0.205642    0.576212    11.00000   -1.50000
H2C   2   -0.063678   -0.122747    0.619344    11.00000   -1.50000
AFIX   0
HKLF 4

REM  p4_nnc in P4/nnc
REM R1 =  0.0466 for     378 Fo > 4sig(Fo)  and  0.0956 for all     774 data
REM     30 parameters refined using      0 restraints

END

WGHT      0.0423      3.1350

REM Highest difference peak  0.544,  deepest hole -0.445,  1-sigma level  0.075
Q1    1   0.1176  0.1329  0.7064  11.00000  0.05    0.54
Q2    1   0.1720  0.1756  0.5271  11.00000  0.05    0.48
Q3    1   0.2500  0.2500  0.5664  10.25000  0.05    0.40
Q4    1   0.3982  0.2500  0.7500  10.50000  0.05    0.29
Q5    1   0.0404  0.0404  0.7500  10.50000  0.05    0.28
Q6    1   0.2467 -0.0572  0.5491  11.00000  0.05    0.22
Q7    1   0.3145  0.1855  0.7500  10.50000  0.05    0.22
Q8    1  -0.2500 -0.2500  0.6482  10.25000  0.05    0.22
Q9    1   0.0211 -0.0483  0.6317  11.00000  0.05    0.22
Q10   1   0.1598 -0.1204  0.5976  11.00000  0.05    0.22
Q11   1   0.0798 -0.2470  0.5777  11.00000  0.05    0.22
Q12   1   0.0084  0.0207  0.5616  11.00000  0.05    0.21
Q13   1   0.1887 -0.1384  0.5997  11.00000  0.05    0.21
Q14   1   0.2427 -0.1158  0.6062  11.00000  0.05    0.20
Q15   1   0.1780 -0.1851  0.5676  11.00000  0.05    0.19
Q16   1   0.0980  0.2359  0.5473  11.00000  0.05    0.19
Q17   1   0.2525  0.1928  0.4809  11.00000  0.05    0.19
Q18   1  -0.0306 -0.0460  0.5713  11.00000  0.05    0.18
Q19   1   0.1556 -0.1152  0.6796  11.00000  0.05    0.18
Q20   1   0.1412 -0.0381  0.6960  11.00000  0.05    0.18
;
_shelx_res_checksum              8492
_database_code_depnum_ccdc_archive 'CCDC 988446'
