#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:30:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180224 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/10/7111048.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111048
loop_
_publ_author_name
'Forbes, Glenn C.'
'Kennedy, Alan R.'
'Mulvey, Robert E.'
'Rowlings, René B.'
'Clegg, William'
'Liddle, Stephen T.'
'Wilson, Chick C.'
_publ_section_title
;
 ‘Inverse crown ether’ complexes extended to group 12
 through the syntheses of [Na2Zn2(HMDS)4(O)] and
 [{K2Zn2(HMDS)4(O2)x(O)y}∞ ]
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1759
_journal_paper_doi               10.1039/b005233g
_journal_year                    2000
_chemical_formula_sum            'C24 H72 K2 N4 O1.82 Si8 Zn2'
_chemical_formula_weight         879.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.322(2)
_cell_angle_beta                 108.154(2)
_cell_angle_gamma                101.162(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9898(4)
_cell_length_b                   10.9763(5)
_cell_length_c                   12.9529(6)
_cell_measurement_reflns_used    9259
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.46
_cell_volume                     1167.11(9)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0112
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10058
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             469
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0047(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0369P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                4753
_reflns_number_total             5263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005233gsup1.cif
_cod_data_source_block           rem294
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111048
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_group
K1 K 0.59619(4) 0.74576(3) 0.56989(2) 0.02930(8) Uani 1 1 d . .
Zn1 Zn 0.617256(17) 0.480649(12) 0.647258(11) 0.01848(5) Uani 1 1 d . .
O1 O 0.5000 0.5000 0.5000 0.018(3) Uani 0.167(7) 2 d SP 1
O2 O 0.4243(2) 0.50474(13) 0.51744(12) 0.0225(5) Uani 0.833(7) 1 d P 2
N1 N 0.75617(12) 0.64066(10) 0.74506(9) 0.0199(2) Uani 1 1 d . .
Si1 Si 0.69505(5) 0.69658(3) 0.85132(3) 0.02441(9) Uani 1 1 d . .
C1 C 0.49117(19) 0.73020(15) 0.79194(14) 0.0378(4) Uani 1 1 d . .
H1A H 0.5035 0.8088 0.7636 0.057 Uiso 1 1 calc R .
H1B H 0.4433 0.7394 0.8500 0.057 Uiso 1 1 calc R .
H1C H 0.4206 0.6599 0.7313 0.057 Uiso 1 1 calc R .
C2 C 0.6867(2) 0.58193(15) 0.94573(12) 0.0371(3) Uani 1 1 d . .
H2A H 0.6316 0.4965 0.9014 0.056 Uiso 1 1 calc R .
H2B H 0.6274 0.6064 0.9937 0.056 Uiso 1 1 calc R .
H2C H 0.7968 0.5829 0.9916 0.056 Uiso 1 1 calc R .
C3 C 0.8275(2) 0.85219(15) 0.94111(14) 0.0427(4) Uani 1 1 d . .
H3A H 0.9377 0.8433 0.9747 0.064 Uiso 1 1 calc R .
H3B H 0.7855 0.8773 0.9997 0.064 Uiso 1 1 calc R .
H3C H 0.8284 0.9171 0.8958 0.064 Uiso 1 1 calc R .
Si2 Si 0.95394(4) 0.68205(3) 0.75159(3) 0.02302(8) Uani 1 1 d . .
C4 C 1.10201(18) 0.66556(17) 0.88429(13) 0.0387(4) Uani 1 1 d . .
H4A H 1.1345 0.7448 0.9391 0.058 Uiso 1 1 calc R .
H4B H 1.1974 0.6471 0.8707 0.058 Uiso 1 1 calc R .
H4C H 1.0517 0.5962 0.9126 0.058 Uiso 1 1 calc R .
C5 C 1.0180(2) 0.85083(15) 0.73687(15) 0.0397(4) Uani 1 1 d . .
H5A H 0.9543 0.8609 0.6633 0.060 Uiso 1 1 calc R .
H5B H 1.1329 0.8714 0.7457 0.060 Uiso 1 1 calc R .
H5C H 1.0002 0.9080 0.7939 0.060 Uiso 1 1 calc R .
C6 C 0.98271(18) 0.58347(15) 0.63430(13) 0.0346(3) Uani 1 1 d . .
H6A H 0.9783 0.4970 0.6472 0.052 Uiso 1 1 calc R .
H6B H 1.0880 0.6201 0.6292 0.052 Uiso 1 1 calc R .
H6C H 0.8969 0.5815 0.5649 0.052 Uiso 1 1 calc R .
N2 N 0.56580(13) 0.30315(9) 0.66299(9) 0.0205(2) Uani 1 1 d . .
Si3 Si 0.40638(5) 0.25458(3) 0.70693(3) 0.02476(9) Uani 1 1 d . .
C7 C 0.30003(18) 0.38267(14) 0.71879(14) 0.0351(3) Uani 1 1 d . .
H7A H 0.3689 0.4509 0.7818 0.053 Uiso 1 1 calc R .
H7B H 0.1987 0.3482 0.7303 0.053 Uiso 1 1 calc R .
H7C H 0.2765 0.4163 0.6505 0.053 Uiso 1 1 calc R .
C8 C 0.2465(2) 0.11786(15) 0.60350(15) 0.0449(4) Uani 1 1 d . .
H8A H 0.1921 0.1477 0.5369 0.067 Uiso 1 1 calc R .
H8B H 0.1672 0.0835 0.6365 0.067 Uiso 1 1 calc R .
H8C H 0.2972 0.0515 0.5834 0.067 Uiso 1 1 calc R .
C9 C 0.4640(2) 0.20204(17) 0.84287(14) 0.0441(4) Uani 1 1 d . .
H9A H 0.5022 0.1248 0.8346 0.066 Uiso 1 1 calc R .
H9B H 0.3697 0.1848 0.8664 0.066 Uiso 1 1 calc R .
H9C H 0.5503 0.2691 0.8988 0.066 Uiso 1 1 calc R .
Si4 Si 0.71721(4) 0.22753(3) 0.67108(3) 0.02244(8) Uani 1 1 d . .
C10 C 0.89716(18) 0.29419(16) 0.79929(13) 0.0373(3) Uani 1 1 d . .
H10A H 0.9454 0.3821 0.7988 0.056 Uiso 1 1 calc R .
H10B H 0.9766 0.2437 0.8021 0.056 Uiso 1 1 calc R .
H10C H 0.8642 0.2918 0.8645 0.056 Uiso 1 1 calc R .
C11 C 0.6553(2) 0.05286(13) 0.66786(14) 0.0375(4) Uani 1 1 d . .
H11A H 0.6326 0.0402 0.7355 0.056 Uiso 1 1 calc R .
H11B H 0.7429 0.0139 0.6634 0.056 Uiso 1 1 calc R .
H11C H 0.5580 0.0135 0.6030 0.056 Uiso 1 1 calc R .
C12 C 0.78103(18) 0.23519(14) 0.54622(12) 0.0325(3) Uani 1 1 d . .
H12A H 0.7018 0.1728 0.4824 0.049 Uiso 1 1 calc R .
H12B H 0.8872 0.2165 0.5616 0.049 Uiso 1 1 calc R .
H12C H 0.7873 0.3203 0.5296 0.049 Uiso 1 1 calc R .
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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 '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
O1 K1 O2 17.12(4) . .
O1 K1 O2 16.43(4) . 2_666
O2 K1 O2 33.55(8) . 2_666
O1 K1 N1 73.83(2) . .
O2 K1 N1 76.54(4) . .
O2 K1 N1 72.59(3) 2_666 .
O1 K1 N2 72.22(2) . 2_666
O2 K1 N2 74.81(4) . 2_666
O2 K1 N2 71.24(3) 2_666 2_666
N1 K1 N2 143.75(3) . 2_666
O1 Zn1 N1 113.35(3) . .
O1 Zn1 N2 111.32(3) . .
N1 Zn1 N2 135.32(4) . .
O1 Zn1 O2 22.30(5) . 2_666
N1 Zn1 O2 109.61(5) . 2_666
N2 Zn1 O2 111.80(5) . 2_666
O1 Zn1 O2 22.17(5) . .
N1 Zn1 O2 113.45(5) . .
N2 Zn1 O2 107.58(5) . .
O2 Zn1 O2 44.47(10) 2_666 .
Zn1 O1 Zn1 180.0 2_666 .
Zn1 O1 K1 88.775(8) 2_666 2_666
Zn1 O1 K1 91.225(8) . 2_666
Zn1 O1 K1 91.225(8) 2_666 .
Zn1 O1 K1 88.775(8) . .
K1 O1 K1 180.0 2_666 .
O2 O2 Zn1 68.17(10) 2_666 2_666
O2 O2 Zn1 67.37(9) 2_666 .
Zn1 O2 Zn1 135.53(10) 2_666 .
O2 O2 K1 77.05(10) 2_666 .
Zn1 O2 K1 86.37(5) 2_666 .
Zn1 O2 K1 83.91(5) . .
O2 O2 K1 69.39(9) 2_666 2_666
Zn1 O2 K1 81.37(5) 2_666 2_666
Zn1 O2 K1 83.32(5) . 2_666
K1 O2 K1 146.45(8) . 2_666
Si2 N1 Si1 122.25(6) . .
Si2 N1 Zn1 118.01(6) . .
Si1 N1 Zn1 115.41(6) . .
Si2 N1 K1 103.00(5) . .
Si1 N1 K1 103.55(5) . .
Zn1 N1 K1 83.07(4) . .
N1 Si1 C2 111.78(6) . .
N1 Si1 C3 114.35(6) . .
C2 Si1 C3 106.66(8) . .
N1 Si1 C1 109.51(6) . .
C2 Si1 C1 110.09(7) . .
C3 Si1 C1 104.13(8) . .
N1 Si2 C6 110.50(6) . .
N1 Si2 C4 113.62(6) . .
C6 Si2 C4 108.18(7) . .
N1 Si2 C5 112.56(6) . .
C6 Si2 C5 105.14(8) . .
C4 Si2 C5 106.36(8) . .
Si4 N2 Si3 124.54(6) . .
Si4 N2 Zn1 115.08(6) . .
Si3 N2 Zn1 117.47(6) . .
Si4 N2 K1 101.05(5) . 2_666
Si3 N2 K1 100.61(5) . 2_666
Zn1 N2 K1 84.14(4) . 2_666
N2 Si3 C7 110.98(6) . .
N2 Si3 C9 114.15(7) . .
C7 Si3 C9 108.17(8) . .
N2 Si3 C8 111.84(7) . .
C7 Si3 C8 104.64(8) . .
C9 Si3 C8 106.51(8) . .
N2 Si4 C10 113.01(6) . .
N2 Si4 C12 110.10(6) . .
C10 Si4 C12 109.19(7) . .
N2 Si4 C11 113.87(6) . .
C10 Si4 C11 106.16(7) . .
C12 Si4 C11 104.03(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.6136(3) .
K1 O2 2.6746(14) .
K1 O2 2.7848(15) 2_666
K1 N1 2.7970(11) .
K1 N2 2.8382(11) 2_666
Zn1 O1 1.93172(16) .
Zn1 N1 1.9614(10) .
Zn1 N2 1.9652(10) .
Zn1 O2 2.0809(15) 2_666
Zn1 O2 2.0928(14) .
O1 Zn1 1.93172(16) 2_666
O1 K1 2.6136(3) 2_666
O2 O2 1.579(4) 2_666
O2 Zn1 2.0809(15) 2_666
O2 K1 2.7848(14) 2_666
N1 Si2 1.7200(11) .
N1 Si1 1.7204(11) .
Si1 C2 1.8701(15) .
Si1 C3 1.8791(15) .
Si1 C1 1.8822(16) .
Si2 C6 1.8655(15) .
Si2 C4 1.8724(15) .
Si2 C5 1.8830(15) .
N2 Si4 1.7098(11) .
N2 Si3 1.7182(11) .
N2 K1 2.8382(11) 2_666
Si3 C7 1.8631(15) .
Si3 C9 1.8728(16) .
Si3 C8 1.8881(16) .
Si4 C10 1.8623(15) .
Si4 C12 1.8832(15) .
Si4 C11 1.8814(14) .
