#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:49:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178669 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/80/4078009.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_4078009
loop_
_publ_author_name
'Michel, Olaf'
'Dietrich, H. Martin'
'Litlabø, Rannveig'
'Törnroos, Karl W.'
'Maichle-Mössmer, Cäcilia'
'Anwander, Reiner'
_publ_section_title
;
 Tris(pyrazolyl)borate Complexes of the Alkaline-Earth Metals:
 Alkylaluminate Precursors and Schlenk-Type Rearrangements
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3119
_journal_paper_doi               10.1021/om300032c
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C24 H60 Al3 Ba K'
_chemical_formula_sum            'C24 H60 Al3 Ba K'
_chemical_formula_weight         606.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.1949(8)
_cell_length_b                   13.1949(8)
_cell_length_c                   32.321(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4873.4(6)
_computing_cell_refinement       X-AREA
_computing_data_collection       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       omega-scans
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            30403
_diffrn_reflns_theta_full        29.07
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         4.76
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  0.83426
_exptl_absorpt_correction_T_min  0.45608
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   mulabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.962
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0427P)²+41.8626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                2796
_reflns_number_total             2878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300032c_si_001.cif
_cod_data_source_block           Compound6
_cod_original_cell_volume        4873.3(6)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4078009
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_assembly
_atom_site_disorder_group
Al1 Al 0.39352(8) 0.05916(8) 0.08320(3) 0.01426(18) Uani 1 1 d . B .
C11 C 0.3470(3) -0.1114(3) 0.07302(10) 0.0186(6) Uani 1 1 d . . .
H11A H 0.2994 -0.1389 0.0475 0.022 Uiso 1 1 calc R . .
H11B H 0.4186 -0.1163 0.0685 0.022 Uiso 1 1 calc R . .
C12 C 0.2770(3) -0.1926(3) 0.10896(11) 0.0258(7) Uani 1 1 d . . .
H12A H 0.2572 -0.2730 0.1024 0.039 Uiso 1 1 calc R . .
H12B H 0.2049 -0.1898 0.1131 0.039 Uiso 1 1 calc R . .
H12C H 0.3242 -0.1670 0.1343 0.039 Uiso 1 1 calc R . .
C13 C 0.4733(3) 0.1483(3) 0.03023(9) 0.0184(6) Uani 1 1 d . . .
H13A H 0.4830 0.2277 0.0316 0.022 Uiso 1 1 calc R . .
H13B H 0.5522 0.1571 0.0284 0.022 Uiso 1 1 calc R . .
C14 C 0.4036(3) 0.0863(3) -0.00883(10) 0.0249(7) Uani 1 1 d . . .
H14A H 0.4450 0.1322 -0.0333 0.037 Uiso 1 1 calc R . .
H14B H 0.3259 0.0787 -0.0074 0.037 Uiso 1 1 calc R . .
H14C H 0.3953 0.0084 -0.0107 0.037 Uiso 1 1 calc R . .
C15 C 0.2478(3) 0.0679(3) 0.09577(11) 0.0247(7) Uani 1 1 d . . .
H15A H 0.1898 -0.0065 0.1090 0.030 Uiso 0.47(9) 1 calc PR A 1
H15B H 0.2683 0.1312 0.1162 0.030 Uiso 0.47(9) 1 calc PR A 1
H15C H 0.1813 -0.0132 0.0978 0.030 Uiso 0.53(9) 1 calc PR A 2
H15D H 0.2579 0.1040 0.1234 0.030 Uiso 0.53(9) 1 calc PR A 2
C16 C 0.1883(19) 0.0905(19) 0.0575(7) 0.040(3) Uani 0.44(3) 1 d PU B 1
H16A H 0.1190 0.0933 0.0667 0.061 Uiso 0.44(3) 1 calc PR B 1
H16B H 0.1651 0.0270 0.0374 0.061 Uiso 0.44(3) 1 calc PR B 1
H16C H 0.2439 0.1651 0.0446 0.061 Uiso 0.44(3) 1 calc PR B 1
C16A C 0.2138(15) 0.1329(16) 0.0664(6) 0.040(3) Uani 0.56(3) 1 d P B 2
H16D H 0.1422 0.1302 0.0763 0.061 Uiso 0.56(3) 1 calc PR B 2
H16E H 0.1998 0.0967 0.0390 0.061 Uiso 0.56(3) 1 calc PR B 2
H16F H 0.2770 0.2145 0.0647 0.061 Uiso 0.56(3) 1 calc PR B 2
C17 C 0.5143(3) 0.1227(3) 0.12858(10) 0.0244(6) Uani 1 1 d . . .
H17A H 0.5562 0.2093 0.1275 0.029 Uiso 1 1 calc R B .
H17B H 0.4740 0.0985 0.1557 0.029 Uiso 1 1 calc R . .
C18 C 0.6038(3) 0.0810(4) 0.12557(12) 0.0323(8) Uani 1 1 d . B .
H18A H 0.6601 0.1147 0.1484 0.048 Uiso 1 1 calc R . .
H18B H 0.6454 0.1063 0.0991 0.048 Uiso 1 1 calc R . .
H18C H 0.5632 -0.0046 0.1273 0.048 Uiso 1 1 calc R . .
Ba1 Ba 0.3333 0.6667 0.032226(9) 0.01539(10) Uani 1 3 d S . .
K1 K 0.0000 0.0000 0.13877(3) 0.01039(18) Uani 1 3 d S . .
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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 '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
C17 Al1 C15 113.97(15) . .
C17 Al1 C11 108.41(14) . .
C15 Al1 C11 108.91(14) . .
C17 Al1 C13 107.30(14) . .
C15 Al1 C13 111.45(14) . .
C11 Al1 C13 106.49(13) . .
C12 C11 Al1 113.1(2) . .
C12 C11 Ba1 86.12(17) . 1_545
Al1 C11 Ba1 160.56(14) . 1_545
C12 C11 H11A 109.0 . .
Al1 C11 H11A 109.0 . .
Ba1 C11 H11A 65.0 1_545 .
C12 C11 H11B 109.0 . .
Al1 C11 H11B 109.0 . .
Ba1 C11 H11B 59.2 1_545 .
H11A C11 H11B 107.8 . .
C11 C12 Ba1 67.04(16) . 1_545
C11 C12 H12A 109.5 . .
Ba1 C12 H12A 42.5 1_545 .
C11 C12 H12B 109.5 . .
Ba1 C12 H12B 127.1 1_545 .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
Ba1 C12 H12C 121.6 1_545 .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 C13 Al1 112.5(2) . .
C14 C13 Ba1 85.72(18) . 10_665
Al1 C13 Ba1 161.44(14) . 10_665
C14 C13 H13A 109.1 . .
Al1 C13 H13A 109.1 . .
Ba1 C13 H13A 65.9 10_665 .
C14 C13 H13B 109.1 . .
Al1 C13 H13B 109.1 . .
Ba1 C13 H13B 58.9 10_665 .
H13A C13 H13B 107.8 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16A C15 C16 21.1(7) . .
C16A C15 Al1 118.2(6) . .
C16 C15 Al1 115.6(8) . .
C16A C15 K1 83.1(6) . .
C16 C15 K1 81.9(8) . .
Al1 C15 K1 157.90(16) . .
C16A C15 H15A 122.6 . .
C16 C15 H15A 108.4 . .
Al1 C15 H15A 108.4 . .
K1 C15 H15A 50.8 . .
C16A C15 H15B 88.4 . .
C16 C15 H15B 108.4 . .
Al1 C15 H15B 108.4 . .
K1 C15 H15B 76.1 . .
H15A C15 H15B 107.5 . .
C16A C15 H15C 107.8 . .
C16 C15 H15C 90.0 . .
Al1 C15 H15C 107.8 . .
K1 C15 H15C 56.4 . .
H15A C15 H15C 21.9 . .
H15B C15 H15C 126.1 . .
C16A C15 H15D 107.8 . .
C16 C15 H15D 125.4 . .
Al1 C15 H15D 107.8 . .
K1 C15 H15D 67.7 . .
H15A C15 H15D 86.5 . .
H15B C15 H15D 22.9 . .
H15C C15 H15D 107.1 . .
C15 C16 K1 70.8(8) . .
C15 C16 H16A 109.5 . .
K1 C16 H16A 41.1 . .
C15 C16 H16B 109.5 . .
K1 C16 H16B 110.6 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
K1 C16 H16C 137.0 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C16A K1 71.1(6) . .
C15 C16A H16D 109.5 . .
K1 C16A H16D 38.9 . .
C15 C16A H16E 109.5 . .
K1 C16A H16E 117.7 . .
H16D C16A H16E 109.5 . .
C15 C16A H16F 109.5 . .
K1 C16A H16F 129.6 . .
H16D C16A H16F 109.5 . .
H16E C16A H16F 109.5 . .
C18 C17 Al1 113.3(2) . .
C18 C17 K1 95.1(2) . 13
Al1 C17 K1 148.19(16) . 13
C18 C17 H17A 108.9 . .
Al1 C17 H17A 108.9 . .
K1 C17 H17A 44.9 13 .
C18 C17 H17B 108.9 . .
Al1 C17 H17B 108.9 . .
K1 C17 H17B 72.6 13 .
H17A C17 H17B 107.7 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C11 Ba1 C11 103.56(7) 1_565 2
C11 Ba1 C11 103.56(7) 1_565 3_665
C11 Ba1 C11 103.56(7) 2 3_665
C11 Ba1 C13 85.52(8) 1_565 11_565
C11 Ba1 C13 84.35(8) 2 11_565
C11 Ba1 C13 165.91(8) 3_665 11_565
C11 Ba1 C13 84.35(8) 1_565 10_665
C11 Ba1 C13 165.91(8) 2 10_665
C11 Ba1 C13 85.52(8) 3_665 10_665
C13 Ba1 C13 84.69(8) 11_565 10_665
C11 Ba1 C13 165.92(8) 1_565 12
C11 Ba1 C13 85.52(8) 2 12
C11 Ba1 C13 84.35(8) 3_665 12
C13 Ba1 C13 84.69(8) 11_565 12
C13 Ba1 C13 84.69(8) 10_665 12
C11 Ba1 C12 26.84(8) 1_565 1_565
C11 Ba1 C12 78.94(8) 2 1_565
C11 Ba1 C12 99.34(9) 3_665 1_565
C13 Ba1 C12 93.58(9) 11_565 1_565
C13 Ba1 C12 110.57(8) 10_665 1_565
C13 Ba1 C12 164.46(8) 12 1_565
C11 Ba1 C12 78.94(8) 1_565 3_665
C11 Ba1 C12 99.34(9) 2 3_665
C11 Ba1 C12 26.84(8) 3_665 3_665
C13 Ba1 C12 164.46(8) 11_565 3_665
C13 Ba1 C12 93.58(9) 10_665 3_665
C13 Ba1 C12 110.57(8) 12 3_665
C12 Ba1 C12 72.53(10) 1_565 3_665
C11 Ba1 C12 99.34(9) 1_565 2
C11 Ba1 C12 26.84(8) 2 2
C11 Ba1 C12 78.94(8) 3_665 2
C13 Ba1 C12 110.57(8) 11_565 2
C13 Ba1 C12 164.46(8) 10_665 2
C13 Ba1 C12 93.57(9) 12 2
C12 Ba1 C12 72.53(10) 1_565 2
C12 Ba1 C12 72.53(10) 3_665 2
C15 K1 C15 102.94(8) 2 .
C15 K1 C15 102.94(8) 2 3
C15 K1 C15 102.94(8) . 3
C15 K1 C17 164.77(10) 2 15_445
C15 K1 C17 86.28(9) . 15_445
C15 K1 C17 86.46(9) 3 15_445
C15 K1 C17 86.28(9) 2 13
C15 K1 C17 86.46(9) . 13
C15 K1 C17 164.77(10) 3 13
C17 K1 C17 82.18(9) 15_445 13
C15 K1 C17 86.45(9) 2 14_455
C15 K1 C17 164.77(10) . 14_455
C15 K1 C17 86.28(9) 3 14_455
C17 K1 C17 82.18(9) 15_445 14_455
C17 K1 C17 82.18(9) 13 14_455
C15 K1 C16 27.3(4) 2 2
C15 K1 C16 93.5(4) . 2
C15 K1 C16 80.4(4) 3 2
C17 K1 C16 166.4(4) 15_445 2
C17 K1 C16 111.4(4) 13 2
C17 K1 C16 100.0(4) 14_455 2
C15 K1 C16 93.5(4) 2 3
C15 K1 C16 80.4(4) . 3
C15 K1 C16 27.3(4) 3 3
C17 K1 C16 100.0(4) 15_445 3
C17 K1 C16 166.4(4) 13 3
C17 K1 C16 111.4(4) 14_455 3
C16 K1 C16 66.6(7) 2 3
C15 K1 C16 80.4(4) 2 .
C15 K1 C16 27.3(4) . .
C15 K1 C16 93.5(4) 3 .
C17 K1 C16 111.4(4) 15_445 .
C17 K1 C16 100.1(4) 13 .
C17 K1 C16 166.4(4) 14_455 .
C16 K1 C16 66.6(7) 2 .
C16 K1 C16 66.6(7) 3 .
C15 K1 C16A 25.8(3) 2 2
C15 K1 C16A 103.0(4) . 2
C15 K1 C16A 77.8(3) 3 2
C17 K1 C16A 163.1(3) 15_445 2
C17 K1 C16A 112.1(3) 13 2
C17 K1 C16A 90.6(4) 14_455 2
C16 K1 C16A 9.6(3) 2 2
C16 K1 C16A 68.3(5) 3 2
C16 K1 C16A 76.1(5) . 2
C15 K1 C16A 103.0(4) 2 3
C15 K1 C16A 77.8(3) . 3
C15 K1 C16A 25.8(3) 3 3
C17 K1 C16A 90.6(4) 15_445 3
C17 K1 C16A 163.1(3) 13 3
C17 K1 C16A 112.1(3) 14_455 3
C16 K1 C16A 76.1(5) 2 3
C16 K1 C16A 9.6(3) 3 3
C16 K1 C16A 68.3(5) . 3
C16A K1 C16A 77.9(5) 2 3
C15 K1 C16A 77.8(3) 2 .
C15 K1 C16A 25.8(3) . .
C15 K1 C16A 103.0(4) 3 .
C17 K1 C16A 112.1(3) 15_445 .
C17 K1 C16A 90.6(4) 13 .
C17 K1 C16A 163.1(3) 14_455 .
C16 K1 C16A 68.3(5) 2 .
C16 K1 C16A 76.1(5) 3 .
C16 K1 C16A 9.6(3) . .
C16A K1 C16A 77.9(5) 2 .
C16A K1 C16A 77.9(5) 3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 C17 2.014(3) .
Al1 C15 2.024(3) .
Al1 C11 2.041(3) .
Al1 C13 2.046(3) .
C11 C12 1.537(4) .
C11 Ba1 3.134(3) 1_545
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 Ba1 3.396(3) 1_545
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C14 1.535(4) .
C13 Ba1 3.211(3) 10_665
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16A 1.490(16) .
C15 C16 1.57(2) .
C15 K1 3.240(3) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C15 H15C 0.9900 .
C15 H15D 0.9900 .
C16 K1 3.40(2) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C16A K1 3.399(16) .
C16A H16D 0.9800 .
C16A H16E 0.9800 .
C16A H16F 0.9800 .
C17 C18 1.536(5) .
C17 K1 3.275(3) 13
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
Ba1 C11 3.134(3) 1_565
Ba1 C11 3.134(3) 2
Ba1 C11 3.134(3) 3_665
Ba1 C13 3.211(3) 11_565
Ba1 C13 3.211(3) 10_665
Ba1 C13 3.211(3) 12
Ba1 C12 3.396(3) 1_565
Ba1 C12 3.396(3) 3_665
Ba1 C12 3.396(3) 2
K1 C15 3.240(3) 2
K1 C15 3.240(3) 3
K1 C17 3.275(3) 15_445
K1 C17 3.275(3) 13
K1 C17 3.275(3) 14_455
K1 C16 3.40(2) 2
K1 C16 3.40(2) 3
K1 C16A 3.399(16) 2
K1 C16A 3.399(16) 3
