#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:33:07 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180267 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/53/7115386.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_7115386
loop_
_publ_author_name
'L. Zane Miller'
'Michael Shatruka'
'D. Tyler McQuade'
_publ_section_title
;
 Alkali metal oxides trapped by diethylzinc
;
_journal_name_full               Chem.Commun.
_journal_page_first              8937
_journal_paper_doi               10.1039/C4cc02929A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '(C2 H5)8 K2 O Zn4'
_chemical_formula_sum            'C16 H40 K2 O Zn4'
_chemical_formula_weight         588.16
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c'
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0272(18)
_cell_length_b                   9.0272(18)
_cell_length_c                   14.145(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1152.7(4)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5225
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.138
_diffrn_reflns_theta_min         2.677
_exptl_absorpt_coefficient_mu    4.473
_exptl_absorpt_correction_T_max  0.454
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0167P)²+0.5855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0380
_refine_ls_wR_factor_ref         0.0430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                483
_reflns_number_total             697
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc02929a3.cif
_cod_data_source_block           added_by_encifer_1
_cod_original_cell_volume        1152.6(5)
_cod_database_code               7115386
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelx_estimated_absorpt_t_min   0.347
_shelx_estimated_absorpt_t_max   0.453
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
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'
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
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_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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
