#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:14:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179318 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/15/4321506.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_4321506
loop_
_publ_author_name
'Timothy J. Boyle'
'Dawn M. Pedrotty'
'Todd M. Alam'
'Sara C. Vick'
'Mark A. Rodriguez'
_publ_section_title
;
 Structural Diversity in Solvated Lithium Aryloxides. Syntheses,
 Characterization, and Structures of [Li(OAr)(THF)x]n and [Li(OAr)(py)x]2
 Complexes Where OAr = OC6H5, OC6H4(2-Me), OC6H3(2,6-(Me))2, OC6H4(2-Pri),
 OC6H3(2,6-(Pri))2, OC6H4(2-But), OC6H3(2,6-(But))2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5133
_journal_page_last               5146
_journal_paper_doi               10.1021/ic000432a
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C18 H29 Li O3'
_chemical_formula_weight         300.35
_chemical_name_common            '[Li(OBP)(THF)2]2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.3260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1510(7)
_cell_length_b                   14.4287(12)
_cell_length_c                   14.1346(12)
_cell_measurement_reflns_used    101
_cell_measurement_temperature    293(2)
_cell_volume                     1799.9(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11255
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0527
_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)+(0.0914P)²+0.1311P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1724
_reflns_number_gt                2494
_reflns_number_total             4149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000432a_6.cif
_cod_data_source_block           tjb036s
_cod_database_code               4321506
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Li1 Li 0.5925(3) 0.00234(19) 0.5840(2) 0.0425(6) Uani 1 1 d . . .
O1 O 0.49701(12) 0.09912(7) 0.49780(8) 0.0403(3) Uani 1 1 d . . .
O2 O 0.56481(18) 0.02408(10) 0.71812(9) 0.0643(4) Uani 1 1 d . . .
O3 O 0.81760(15) -0.01717(9) 0.63525(10) 0.0591(4) Uani 1 1 d . . .
C1 C 0.42430(17) 0.17105(11) 0.52153(11) 0.0362(4) Uani 1 1 d . . .
C2 C 0.46437(17) 0.26469(11) 0.50810(11) 0.0373(4) Uani 1 1 d . . .
C3 C 0.3802(2) 0.33455(12) 0.53786(13) 0.0497(5) Uani 1 1 d . . .
H3 H 0.4055 0.3960 0.5300 0.060 Uiso 1 1 calc R . .
C4 C 0.2609(2) 0.31660(16) 0.57853(14) 0.0601(6) Uani 1 1 d . . .
H4 H 0.2078 0.3652 0.5972 0.072 Uiso 1 1 calc R . .
C5 C 0.2218(2) 0.22665(16) 0.59087(13) 0.0562(5) Uani 1 1 d . . .
H5 H 0.1422 0.2135 0.6182 0.067 Uiso 1 1 calc R . .
C6 C 0.3016(2) 0.15590(14) 0.56245(13) 0.0496(5) Uani 1 1 d . . .
H6 H 0.2732 0.0952 0.5706 0.060 Uiso 1 1 calc R . .
C7 C 0.59535(19) 0.28728(11) 0.46401(13) 0.0460(4) Uani 1 1 d . . .
C8 C 0.7440(2) 0.24827(14) 0.52909(17) 0.0635(6) Uani 1 1 d . . .
H8A H 0.7634 0.2750 0.5934 0.095 Uiso 1 1 calc R . .
H8B H 0.8257 0.2632 0.5009 0.095 Uiso 1 1 calc R . .
H8C H 0.7360 0.1822 0.5337 0.095 Uiso 1 1 calc R . .
C9 C 0.5656(2) 0.24571(14) 0.36078(14) 0.0595(5) Uani 1 1 d . . .
H9A H 0.5553 0.1797 0.3644 0.089 Uiso 1 1 calc R . .
H9B H 0.6488 0.2600 0.3338 0.089 Uiso 1 1 calc R . .
H9C H 0.4739 0.2714 0.3196 0.089 Uiso 1 1 calc R . .
C10 C 0.6168(3) 0.39240(13) 0.45477(19) 0.0711(7) Uani 1 1 d . . .
H10A H 0.5250 0.4191 0.4148 0.107 Uiso 1 1 calc R . .
H10B H 0.6980 0.4036 0.4249 0.107 Uiso 1 1 calc R . .
H10C H 0.6408 0.4201 0.5188 0.107 Uiso 1 1 calc R . .
C11 C 0.6125(3) 0.11235(17) 0.76300(16) 0.0786(7) Uani 1 1 d . . .
H11A H 0.5940 0.1613 0.7142 0.094 Uiso 1 1 calc R . .
H11B H 0.7195 0.1115 0.7969 0.094 Uiso 1 1 calc R . .
C12 C 0.5194(3) 0.12608(16) 0.83311(15) 0.0751(7) Uani 1 1 d . . .
H12A H 0.4192 0.1489 0.8002 0.090 Uiso 1 1 calc R . .
H12B H 0.5676 0.1689 0.8849 0.090 Uiso 1 1 calc R . .
C13 C 0.5124(3) 0.03059(16) 0.87224(16) 0.0692(6) Uani 1 1 d . . .
H13A H 0.5979 0.0188 0.9283 0.083 Uiso 1 1 calc R . .
H13B H 0.4192 0.0212 0.8913 0.083 Uiso 1 1 calc R . .
C14 C 0.5181(3) -0.03002(15) 0.78792(14) 0.0602(5) Uani 1 1 d . . .
H14A H 0.5890 -0.0804 0.8102 0.072 Uiso 1 1 calc R . .
H14B H 0.4189 -0.0563 0.7588 0.072 Uiso 1 1 calc R . .
C15 C 0.9480(2) 0.03308(16) 0.63055(19) 0.0740(7) Uani 1 1 d . . .
H15A H 0.9529 0.0915 0.6653 0.089 Uiso 1 1 calc R . .
H15B H 0.9461 0.0459 0.5629 0.089 Uiso 1 1 calc R . .
C16 C 1.0830(3) -0.02721(18) 0.6784(2) 0.0845(8) Uani 1 1 d . . .
H16A H 1.1603 -0.0237 0.6429 0.101 Uiso 1 1 calc R . .
H16B H 1.1269 -0.0088 0.7459 0.101 Uiso 1 1 calc R . .
C17 C 1.0181(2) -0.12174(15) 0.67294(16) 0.0653(6) Uani 1 1 d . . .
H17A H 1.0772 -0.1611 0.7247 0.078 Uiso 1 1 calc R . .
H17B H 1.0117 -0.1503 0.6099 0.078 Uiso 1 1 calc R . .
C18 C 0.8653(2) -0.10312(15) 0.68646(16) 0.0654(6) Uani 1 1 d . . .
H18A H 0.7958 -0.1528 0.6588 0.079 Uiso 1 1 calc R . .
H18B H 0.8700 -0.0970 0.7555 0.079 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'
Li Li -0.0003 0.0001 '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'
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
O1 Li1 O1 97.10(13) . 3_656 ?
O1 Li1 O2 109.81(14) . . ?
O1 Li1 O2 123.47(15) 3_656 . ?
O1 Li1 O3 125.77(15) . . ?
O1 Li1 O3 110.16(14) 3_656 . ?
O2 Li1 O3 93.14(13) . . ?
O1 Li1 Li1 48.61(10) . 3_656 ?
O1 Li1 Li1 48.48(10) 3_656 3_656 ?
O2 Li1 Li1 132.3(2) . 3_656 ?
O3 Li1 Li1 134.56(19) . 3_656 ?
C1 O1 Li1 126.08(13) . . ?
C1 O1 Li1 126.19(13) . 3_656 ?
Li1 O1 Li1 82.90(13) . 3_656 ?
C14 O2 C11 107.11(15) . . ?
C14 O2 Li1 135.50(15) . . ?
C11 O2 Li1 117.17(14) . . ?
C15 O3 C18 108.48(15) . . ?
C15 O3 Li1 135.02(15) . . ?
C18 O3 Li1 116.45(14) . . ?
O1 C1 C6 119.40(15) . . ?
O1 C1 C2 123.05(14) . . ?
C6 C1 C2 117.55(15) . . ?
C3 C2 C1 117.47(16) . . ?
C3 C2 C7 121.56(15) . . ?
C1 C2 C7 120.97(14) . . ?
C4 C3 C2 123.14(18) . . ?
C5 C4 C3 119.37(18) . . ?
C4 C5 C6 119.32(18) . . ?
C5 C6 C1 123.14(18) . . ?
C2 C7 C8 110.17(15) . . ?
C2 C7 C9 110.11(14) . . ?
C8 C7 C9 109.48(16) . . ?
C2 C7 C10 112.14(15) . . ?
C8 C7 C10 107.44(16) . . ?
C9 C7 C10 107.41(16) . . ?
O2 C11 C12 104.64(18) . . ?
C11 C12 C13 102.32(18) . . ?
C14 C13 C12 103.37(17) . . ?
O2 C14 C13 108.42(18) . . ?
O3 C15 C16 106.47(18) . . ?
C17 C16 C15 103.70(19) . . ?
C16 C17 C18 101.83(18) . . ?
O3 C18 C17 105.14(17) . . ?
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
Li1 O1 1.907(3) . ?
Li1 O1 1.911(3) 3_656 ?
Li1 O2 2.002(3) . ?
Li1 O3 2.014(3) . ?
Li1 Li1 2.527(6) 3_656 ?
O1 C1 1.3230(19) . ?
O1 Li1 1.911(3) 3_656 ?
O2 C14 1.410(2) . ?
O2 C11 1.438(2) . ?
O3 C15 1.413(3) . ?
O3 C18 1.444(2) . ?
C1 C6 1.409(2) . ?
C1 C2 1.426(2) . ?
C2 C3 1.399(2) . ?
C2 C7 1.525(2) . ?
C3 C4 1.386(3) . ?
C4 C5 1.369(3) . ?
C5 C6 1.375(3) . ?
C7 C8 1.534(3) . ?
C7 C9 1.534(3) . ?
C7 C10 1.539(3) . ?
C11 C12 1.481(3) . ?
C12 C13 1.492(3) . ?
C13 C14 1.490(3) . ?
C15 C16 1.516(3) . ?
C16 C17 1.481(3) . ?
C17 C18 1.485(3) . ?
