#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:49:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178669 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/80/4078010.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_4078010
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         'C8 H20 Al K'
_chemical_formula_sum            'C8 H20 Al K'
_chemical_formula_weight         182.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_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            3
_cell_length_a                   7.3108(4)
_cell_length_b                   7.3108(4)
_cell_length_c                   17.6876(13)
_cell_measurement_reflns_used    13743
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      3.12
_cell_volume                     818.71(9)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14997
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         4.72
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.26(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0223
_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)+(0.0248P)²+0.1278P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                1447
_reflns_number_total             1464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300032c_si_001.cif
_cod_data_source_block           Compound7
_cod_original_sg_symbol_H-M      P3121
_cod_database_code               4078010
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'-x, -x+y, -z+1/3'
'x-y, -y, -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
K K 0.45173(5) 0.0000 0.3333 0.03136(11) Uani 1 2 d S
Al Al 0.0000 0.16368(6) 0.1667 0.01699(10) Uani 1 2 d S
C11 C 0.09606(17) 0.37384(17) 0.08123(6) 0.02153(19) Uani 1 1 d .
H11A H 0.2246 0.5052 0.0970 0.026 Uiso 1 1 calc R
H11B H 0.1332 0.3155 0.0371 0.026 Uiso 1 1 calc R
C12 C -0.0749(2) 0.4265(2) 0.05791(7) 0.0291(3) Uani 1 1 d .
H12A H -0.2027 0.2967 0.0425 0.044 Uiso 1 1 calc R
H12B H -0.0234 0.5262 0.0155 0.044 Uiso 1 1 calc R
H12C H -0.1076 0.4901 0.1008 0.044 Uiso 1 1 calc R
C15 C 0.22391(18) 0.10778(17) 0.20796(6) 0.0213(2) Uani 1 1 d .
H15A H 0.1505 -0.0017 0.2483 0.026 Uiso 1 1 d R
H15B H 0.3377 0.2317 0.2326 0.026 Uiso 1 1 d R
C16 C 0.3253(2) 0.0289(2) 0.15045(7) 0.0307(3) Uani 1 1 d .
H16A H 0.2149 -0.0969 0.1248 0.046 Uiso 1 1 calc R
H16B H 0.4215 -0.0068 0.1766 0.046 Uiso 1 1 calc R
H16C H 0.4045 0.1398 0.1131 0.046 Uiso 1 1 calc R
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
K 0.02513(13) 0.0438(2) 0.03140(18) 0.01570(16) 0.00785(8) 0.02189(12)
Al 0.0174(2) 0.01689(15) 0.01685(18) -0.00083(7) -0.00166(15) 0.00870(11)
C11 0.0209(5) 0.0236(5) 0.0202(4) 0.0012(4) 0.0022(4) 0.0112(4)
C12 0.0282(6) 0.0322(6) 0.0284(5) 0.0080(5) 0.0003(5) 0.0163(5)
C15 0.0209(5) 0.0214(5) 0.0221(4) -0.0004(4) -0.0027(4) 0.0110(4)
C16 0.0314(6) 0.0387(7) 0.0284(5) -0.0032(5) -0.0015(5) 0.0224(5)
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'
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
C15 Al C15 104.84(7) . 5
C15 Al C11 107.41(4) . 5
C15 Al C11 114.73(4) 5 5
C15 Al C11 114.73(4) . .
C15 Al C11 107.41(4) 5 .
C11 Al C11 107.92(6) 5 .
C12 C11 Al 112.05(7) . .
C12 C11 H11A 109.2 . .
Al C11 H11A 109.2 . .
C12 C11 H11B 109.2 . .
Al C11 H11B 109.2 . .
H11A C11 H11B 107.9 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C16 C15 Al 115.57(7) . .
C16 C15 H15A 109.8 . .
Al C15 H15A 104.8 . .
C16 C15 H15B 107.4 . .
Al C15 H15B 112.1 . .
H15A C15 H15B 106.9 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al C15 2.0123(11) .
Al C15 2.0123(11) 5
Al C11 2.0146(11) 5
Al C11 2.0146(11) .
C11 C12 1.5367(16) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C15 C16 1.5315(16) .
C15 H15A 1.0041 .
C15 H15B 0.9745 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
