#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:40:15 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229926 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/65/7046525.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_7046525
loop_
_publ_author_name
'Kaiser, Maximillian'
'Klett, Jan'
_publ_section_title
;
 The hetero-cubane structures of the heavy alkali metal tert-amyloxides
 [MOCMe₂Et]₄ (M = K, Rb, Cs).
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12582
_journal_page_last               12586
_journal_paper_doi               10.1039/c8dt01545g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C5 H11 K O'
_chemical_formula_weight         126.24
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-05-30 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.2509(4)
_cell_length_b                   8.2509(4)
_cell_length_c                   20.346(3)
_cell_measurement_reflns_used    5019
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.8242
_cell_measurement_theta_min      2.4685
_cell_volume                     1385.1(2)
_computing_cell_refinement       APEX2
_computing_data_collection       APEX2
_computing_data_reduction        APEX2
_computing_molecular_graphics    ShelXP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    ShelXS
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7105
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.869
_diffrn_reflns_theta_min         2.002
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  1.0709
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0222
_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)+(0.0274P)²+0.1681P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1629
_reflns_number_total             1664
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01545g2.cif
_cod_data_source_block           JKM5
_cod_depositor_comments
'Adding full bibliography for 7046525--7046528.cif.'
_cod_database_code               7046525
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, 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
K1 K 0.36257(4) 0.32344(4) 0.06376(2) 0.02379(12) Uani 1 1 d . .
O1 O 0.68036(14) 0.36232(14) 0.06413(6) 0.0248(3) Uani 1 1 d . .
C10 C 0.7765(2) 0.2731(2) 0.10649(8) 0.0191(3) Uani 1 1 d . .
C11 C 0.9466(2) 0.2478(2) 0.07659(10) 0.0292(4) Uani 1 1 d . .
H11A H 1.0157(11) 0.1910(17) 0.1083(5) 0.044 Uiso 1 1 calc R U
H11B H 0.9947(10) 0.3534(14) 0.0661(6) 0.044 Uiso 1 1 calc R U
H11C H 0.9376(3) 0.1831(17) 0.0363(7) 0.044 Uiso 1 1 calc R U
C12 C 0.7017(3) 0.1050(2) 0.11848(9) 0.0290(4) Uani 1 1 d . .
H12A H 0.5987(16) 0.1172(3) 0.1401(7) 0.044 Uiso 1 1 calc R U
H12B H 0.7731(13) 0.0419(11) 0.1457(7) 0.044 Uiso 1 1 calc R U
H12C H 0.6864(17) 0.0508(11) 0.0771(6) 0.044 Uiso 1 1 calc R U
C13 C 0.7916(2) 0.3641(2) 0.17279(8) 0.0282(4) Uani 1 1 d . .
H13A H 0.8440 0.4672 0.1643 0.034 Uiso 1 1 calc R U
H13B H 0.6829 0.3874 0.1883 0.034 Uiso 1 1 calc R U
C14 C 0.8833(3) 0.2806(3) 0.22842(10) 0.0507(6) Uani 1 1 d . .
H14A H 0.889(2) 0.3518(15) 0.2658(7) 0.076 Uiso 1 1 calc R U
H14B H 0.991(2) 0.255(2) 0.2140(4) 0.076 Uiso 1 1 calc R U
H14C H 0.8278(17) 0.182(2) 0.2405(7) 0.076 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'
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 O1 90.84(4) 3_565 2_665
O1 K1 O1 90.29(4) 3_565 .
O1 K1 O1 90.80(4) 2_665 .
O1 K1 C11 94.11(4) 3_565 1_455
O1 K1 C11 92.50(4) 2_665 1_455
O1 K1 C11 174.45(4) . 1_455
O1 K1 C12 108.16(4) 3_565 .
O1 K1 C12 128.01(4) 2_665 .
O1 K1 C12 43.12(4) . .
C11 K1 C12 131.84(5) 1_455 .
O1 K1 K1 45.86(3) 3_565 3_565
O1 K1 K1 44.99(3) 2_665 3_565
O1 K1 K1 90.21(3) . 3_565
C11 K1 K1 95.28(3) 1_455 3_565
C12 K1 K1 130.92(3) . 3_565
O1 K1 K1 45.31(3) 3_565 4_655
O1 K1 K1 90.60(3) 2_665 4_655
O1 K1 K1 44.99(3) . 4_655
C11 K1 K1 139.36(4) 1_455 4_655
C12 K1 K1 72.99(3) . 4_655
K1 K1 K1 60.203(13) 3_565 4_655
O1 K1 K1 90.57(3) 3_565 2_665
O1 K1 K1 45.68(3) 2_665 2_665
O1 K1 K1 45.13(3) . 2_665
C11 K1 K1 138.02(4) 1_455 2_665
C12 K1 K1 85.15(3) . 2_665
K1 K1 K1 59.899(7) 3_565 2_665
K1 K1 K1 59.899(7) 4_655 2_665
C10 O1 K1 129.06(10) . 4_655
C10 O1 K1 127.35(9) . 2_665
K1 O1 K1 89.70(4) 4_655 2_665
C10 O1 K1 120.43(9) . .
K1 O1 K1 89.16(4) 4_655 .
K1 O1 K1 89.19(4) 2_665 .
O1 C10 C12 110.39(14) . .
O1 C10 C11 110.35(13) . .
C12 C10 C11 107.82(15) . .
O1 C10 C13 109.29(14) . .
C12 C10 C13 109.34(14) . .
C11 C10 C13 109.63(15) . .
C10 C11 K1 153.81(13) . 1_655
C10 C12 K1 78.86(10) . .
C14 C13 C10 117.83(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.6023(12) 3_565
K1 O1 2.6168(12) 2_665
K1 O1 2.6416(12) .
K1 C11 3.498(2) 1_455
K1 C12 3.509(2) .
K1 K1 3.6808(7) 3_565
K1 K1 3.6808(7) 4_655
K1 K1 3.6921(7) 2_665
O1 C10 1.384(2) .
O1 K1 2.6024(12) 4_655
O1 K1 2.6169(12) 2_665
C10 C12 1.537(2) .
C10 C11 1.544(2) .
C10 C13 1.549(2) .
C11 K1 3.498(2) 1_655
C13 C14 1.526(3) .
