#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179312 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/09/4320902.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_4320902
loop_
_publ_author_name
'Witold Paw'
'Thomas H. Baum'
'Kin-Chung Lam'
'Arnold L. Rheingold'
_publ_section_title
;
 Low-Melting, Mononuclear Tetrahydrofuran Complexes of
 M(2,2,6,6-tetramethylheptane-3,5-dionate)2 (M = Ba, Sr) and Related
 Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2011
_journal_page_last               2014
_journal_paper_doi               10.1021/ic990641z
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C38 H70 Ba O8'
_chemical_formula_weight         792.28
_chemical_name_systematic
;
 [Ba(thd)2(THF)4]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 109.3710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9003(4)
_cell_length_b                   9.5492(2)
_cell_length_c                   23.6351(4)
_cell_measurement_reflns_used    3977
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     4237.17(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9593
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.560
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.560
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2291
_reflns_number_gt                2603
_reflns_number_total             3283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990641z_1.cif
_cod_data_source_block           atm22r1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4237.15(15)
_cod_database_code               4320902
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.2500 0.50739(7) 0.0000 0.0374(3) Uani 1 2 d S . .
O1 O 0.3204(3) 0.5639(8) 0.1145(3) 0.0520(16) Uani 1 1 d . . .
O2 O 0.1804(3) 0.4490(8) 0.0749(3) 0.0509(16) Uani 1 1 d . . .
O3 O 0.3272(3) 0.7501(8) -0.0012(4) 0.068(2) Uani 1 1 d . . .
O4 O 0.3291(3) 0.2643(7) 0.0434(3) 0.063(2) Uani 1 1 d . . .
C1 C 0.3119(4) 0.5579(9) 0.1642(4) 0.0356(17) Uani 1 1 d . . .
C2 C 0.2509(5) 0.5032(8) 0.1741(4) 0.0367(18) Uani 1 1 d . . .
H2A H 0.2507 0.5026 0.2142 0.044 Uiso 1 1 calc R . .
C3 C 0.1911(4) 0.4500(9) 0.1301(4) 0.0383(19) Uani 1 1 d . . .
C4 C 0.3728(4) 0.6156(8) 0.2161(4) 0.043(2) Uani 1 1 d . . .
C5 C 0.3980(7) 0.7523(14) 0.1988(5) 0.100(5) Uani 1 1 d . . .
H5A H 0.4092 0.7397 0.1617 0.150 Uiso 1 1 calc R . .
H5B H 0.4408 0.7833 0.2309 0.150 Uiso 1 1 calc R . .
H5C H 0.3605 0.8229 0.1923 0.150 Uiso 1 1 calc R . .
C6 C 0.3560(5) 0.6357(11) 0.2742(4) 0.057(3) Uani 1 1 d . . .
H6A H 0.3175 0.7042 0.2676 0.086 Uiso 1 1 calc R . .
H6B H 0.3986 0.6696 0.3058 0.086 Uiso 1 1 calc R . .
H6C H 0.3411 0.5460 0.2865 0.086 Uiso 1 1 calc R . .
C7 C 0.4343(6) 0.5083(12) 0.2308(6) 0.074(4) Uani 1 1 d . . .
H7A H 0.4472 0.4909 0.1948 0.111 Uiso 1 1 calc R . .
H7B H 0.4191 0.4205 0.2443 0.111 Uiso 1 1 calc R . .
H7C H 0.4757 0.5456 0.2627 0.111 Uiso 1 1 calc R . .
C8 C 0.1286(4) 0.3891(9) 0.1471(4) 0.043(2) Uani 1 1 d . . .
C9 C 0.0622(5) 0.4727(11) 0.1156(6) 0.065(3) Uani 1 1 d . . .
H9A H 0.0690 0.5698 0.1297 0.098 Uiso 1 1 calc R . .
H9B H 0.0216 0.4319 0.1245 0.098 Uiso 1 1 calc R . .
H9C H 0.0530 0.4704 0.0722 0.098 Uiso 1 1 calc R . .
C10 C 0.1410(5) 0.3859(12) 0.2146(5) 0.064(3) Uani 1 1 d . . .
H10A H 0.1473 0.4817 0.2303 0.096 Uiso 1 1 calc R . .
H10B H 0.1837 0.3308 0.2348 0.096 Uiso 1 1 calc R . .
H10C H 0.0997 0.3431 0.2217 0.096 Uiso 1 1 calc R . .
C11 C 0.1183(6) 0.2357(10) 0.1248(5) 0.066(3) Uani 1 1 d . . .
H11A H 0.1102 0.2333 0.0816 0.100 Uiso 1 1 calc R . .
H11B H 0.0771 0.1952 0.1329 0.100 Uiso 1 1 calc R . .
H11C H 0.1611 0.1814 0.1459 0.100 Uiso 1 1 calc R . .
C12 C 0.4020(5) 0.7390(16) 0.0204(7) 0.088(4) Uani 1 1 d . . .
H12A H 0.4161 0.6419 0.0148 0.105 Uiso 1 1 calc R . .
H12B H 0.4200 0.7604 0.0638 0.105 Uiso 1 1 calc R . .
C13 C 0.4327(8) 0.8342(18) -0.0110(9) 0.123(6) Uani 1 1 d . . .
H13A H 0.4593 0.9094 0.0161 0.147 Uiso 1 1 calc R . .
H13B H 0.4655 0.7845 -0.0278 0.147 Uiso 1 1 calc R . .
C14 C 0.3760(11) 0.888(3) -0.0556(9) 0.159(9) Uani 1 1 d . . .
H14A H 0.3730 0.9897 -0.0493 0.191 Uiso 1 1 calc R . .
H14B H 0.3834 0.8737 -0.0946 0.191 Uiso 1 1 calc R . .
C15 C 0.3135(7) 0.8262(15) -0.0574(7) 0.111(6) Uani 1 1 d . . .
H15A H 0.2970 0.7611 -0.0918 0.133 Uiso 1 1 calc R . .
H15B H 0.2763 0.8982 -0.0617 0.133 Uiso 1 1 calc R . .
C16 C 0.3109(6) 0.1891(15) 0.0897(7) 0.103(6) Uani 1 1 d . . .
H16A H 0.2945 0.2552 0.1147 0.123 Uiso 1 1 calc R . .
H16B H 0.2724 0.1207 0.0715 0.123 Uiso 1 1 calc R . .
C17 C 0.3733(9) 0.120(2) 0.1249(8) 0.140(8) Uani 1 1 d . . .
H17A H 0.3694 0.0182 0.1156 0.168 Uiso 1 1 calc R . .
H17B H 0.3796 0.1312 0.1680 0.168 Uiso 1 1 calc R . .
C18 C 0.4335(7) 0.1782(16) 0.1121(7) 0.101(5) Uani 1 1 d . . .
H18A H 0.4613 0.1033 0.1011 0.122 Uiso 1 1 calc R . .
H18B H 0.4651 0.2287 0.1475 0.122 Uiso 1 1 calc R . .
C19 C 0.4033(5) 0.2764(16) 0.0609(6) 0.086(4) Uani 1 1 d . . .
H19A H 0.4182 0.3737 0.0735 0.104 Uiso 1 1 calc R . .
H19B H 0.4202 0.2515 0.0273 0.104 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'
O O 0.0106 0.0060 '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'
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
_geom_angle_publ_flag
O2 Ba1 O2 155.6(3) . 2 ?
O2 Ba1 O1 120.5(2) . 2 ?
O2 Ba1 O1 65.02(18) 2 2 ?
O2 Ba1 O1 65.02(18) . . ?
O2 Ba1 O1 120.5(2) 2 . ?
O1 Ba1 O1 156.6(3) 2 . ?
O2 Ba1 O3 75.9(2) . 2 ?
O2 Ba1 O3 126.5(2) 2 2 ?
O1 Ba1 O3 74.6(2) 2 2 ?
O1 Ba1 O3 85.8(2) . 2 ?
O2 Ba1 O3 126.5(2) . . ?
O2 Ba1 O3 75.9(2) 2 . ?
O1 Ba1 O3 85.8(2) 2 . ?
O1 Ba1 O3 74.6(2) . . ?
O3 Ba1 O3 67.4(3) 2 . ?
O2 Ba1 O4 73.4(2) . 2 ?
O2 Ba1 O4 86.3(2) 2 2 ?
O1 Ba1 O4 75.7(2) 2 2 ?
O1 Ba1 O4 125.7(2) . 2 ?
O3 Ba1 O4 116.65(19) 2 2 ?
O3 Ba1 O4 158.5(3) . 2 ?
O2 Ba1 O4 86.3(2) . . ?
O2 Ba1 O4 73.4(2) 2 . ?
O1 Ba1 O4 125.7(2) 2 . ?
O1 Ba1 O4 75.7(2) . . ?
O3 Ba1 O4 158.5(3) 2 . ?
O3 Ba1 O4 116.65(19) . . ?
O4 Ba1 O4 68.1(3) 2 . ?
C1 O1 Ba1 139.6(5) . . ?
C3 O2 Ba1 138.7(5) . . ?
C12 O3 C15 102.9(9) . . ?
C12 O3 Ba1 117.0(7) . . ?
C15 O3 Ba1 119.1(7) . . ?
C19 O4 C16 108.6(8) . . ?
C19 O4 Ba1 116.7(7) . . ?
C16 O4 Ba1 115.8(6) . . ?
O1 C1 C2 124.7(8) . . ?
O1 C1 C4 115.2(7) . . ?
C2 C1 C4 120.1(8) . . ?
C3 C2 C1 125.6(8) . . ?
O2 C3 C2 126.2(8) . . ?
O2 C3 C8 113.3(7) . . ?
C2 C3 C8 120.5(8) . . ?
C5 C4 C1 110.1(8) . . ?
C5 C4 C6 109.2(8) . . ?
C1 C4 C6 114.7(7) . . ?
C5 C4 C7 109.0(10) . . ?
C1 C4 C7 107.6(7) . . ?
C6 C4 C7 105.9(8) . . ?
C9 C8 C10 109.6(8) . . ?
C9 C8 C3 108.8(7) . . ?
C10 C8 C3 114.5(7) . . ?
C9 C8 C11 109.7(8) . . ?
C10 C8 C11 107.0(8) . . ?
C3 C8 C11 107.2(7) . . ?
O3 C12 C13 110.2(11) . . ?
C14 C13 C12 104.6(13) . . ?
C15 C14 C13 112.0(16) . . ?
C14 C15 O3 107.1(12) . . ?
C17 C16 O4 106.7(10) . . ?
C16 C17 C18 108.8(12) . . ?
C17 C18 C19 106.0(10) . . ?
O4 C19 C18 106.8(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 O2 2.643(6) . ?
Ba1 O2 2.644(6) 2 ?
Ba1 O1 2.657(6) 2 ?
Ba1 O1 2.657(6) . ?
Ba1 O3 2.786(7) 2 ?
Ba1 O3 2.786(7) . ?
Ba1 O4 2.801(6) 2 ?
Ba1 O4 2.801(6) . ?
O1 C1 1.243(10) . ?
O2 C3 1.251(11) . ?
O3 C12 1.408(11) . ?
O3 C15 1.458(15) . ?
O4 C19 1.401(10) . ?
O4 C16 1.452(12) . ?
C1 C2 1.409(12) . ?
C1 C4 1.515(11) . ?
C2 C3 1.391(12) . ?
C3 C8 1.541(11) . ?
C4 C5 1.503(14) . ?
C4 C6 1.529(13) . ?
C4 C7 1.546(13) . ?
C8 C9 1.511(13) . ?
C8 C10 1.532(13) . ?
C8 C11 1.547(12) . ?
C12 C13 1.432(18) . ?
C13 C14 1.36(2) . ?
C14 C15 1.36(2) . ?
C16 C17 1.410(17) . ?
C17 C18 1.443(19) . ?
C18 C19 1.491(16) . ?
